CN108854600A - Graphene oxide/polyurethane hollow fiber ultrafiltration membrane and preparation method thereof - Google Patents
Graphene oxide/polyurethane hollow fiber ultrafiltration membrane and preparation method thereof Download PDFInfo
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- CN108854600A CN108854600A CN201810616582.4A CN201810616582A CN108854600A CN 108854600 A CN108854600 A CN 108854600A CN 201810616582 A CN201810616582 A CN 201810616582A CN 108854600 A CN108854600 A CN 108854600A
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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
- B01D71/60—Polyamines
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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
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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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
- B01D69/08—Hollow fibre 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/48—Antimicrobial properties
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of graphene oxide/polyurethane hollow fiber ultrafiltration membrane and preparation method thereof, the formula and its content of film by percentage to the quality, including：Polyurethane 25~50%, chliorinated polyvinyl chloride 2~10%, graphene oxide 1~5%, polyethylene glycol/polyvinylpyrrolidone mixture 5~10%, Tween-80 1~5%, dimethyl acetamide 20%~66%.Above-mentioned each component is configured to homogeneous casting solution, casting solution and composite braided pipe Jing Guo the pre-heat treatment are passed through and coated using spinneret die, coagulating bath is entered after air section, the filter membrane is made.The coating that casting solution of the invention is formed firmly is attached to braiding pipe surface, and film wire flux is higher, and toughness and shock resistance are good, is suitable for higher pressure backwash；Graphene/polyurethane composite hollow fiber membrane made from after composite modified has the function of catalysis, antibacterial etc..
Description
Technical field
The present invention relates to fibrous filter membrane preparation fields, and in particular to a kind of graphene oxide/polyurethane hollow fiber ultrafiltration
Film and preparation method thereof.
Background technique
Membrane biological reactor process (MBR) is a kind of novel, efficient sewage disposal technology, it can be realized simultaneously biology
Catalysis reaction and the separation of water and degradation material, are regenerated water resource, realize reuse water standard.MBR technology is the present age
Advanced, efficient and low energy consumption Sewage advanced treatment and regeneration new technology.Wherein, preparation intensity is high, contamination resistance is strong,
The ultrafiltration membrane of low cost is the core technology of membrane biological reactor process.Compared to Kynoar (PVDF), polyvinyl chloride
(PVC), polypropylene (PP), polysulfones (PSF) and polyacrylonitrile (PAN), polyurethane (PUR) mechanical strength with higher, stabilization
Chemical property, corrosion-resistant and antifouling property it is good, become a kind of more preferably membrane material.Currently, having high-strength
The modified PUR hollow-fibre membrane of the graphene that the crocheted network management of degree, catalysis and antibacterial action is reinforced also is rarely reported.
Summary of the invention
The purpose of the present invention is to propose to a kind of graphene oxide/polyurethane suitable for applying in membrane biological reactor process
Hollow fiber ultrafiltration membrane and preparation method thereof.
The purpose of the present invention is achieved through the following technical solutions：
In a first aspect, the present invention relates to a kind of graphene oxide/polyurethane hollow fiber ultrafiltration membrane, the formula of film and
Its content by percentage to the quality, including：
Preferably, polyurethane (PUR) weight average molecular weight is 350000, and the chliorinated polyvinyl chloride (CPVC) is divided equally again
Son amount is 65000.
On the other hand, the invention further relates to the graphene oxide/polyurethane hollow fiber ultrafiltration membrane preparation method,
Described method includes following steps：
The pretreatment of S1, polymer material：By polyurethane, chliorinated polyvinyl chloride, graphene oxide in 60~80 DEG C of vacuum
Dry 12~15h；
The preparation of S2, casting solution：By polyurethane (P1), chliorinated polyvinyl chloride (P2), it is graphene oxide, pore-foaming agent, hydrophilic
Agent, solvent after weighing proportionally, are first placed in stirred tank, 80~100 DEG C at a temperature of be stirred dissolution, mixing time
For 15~for 24 hours, speed of agitator is 80~120 revs/min, after acquired solution vacuumizing and defoaming, stands 1h or more, obtains spinning and casts
Film liquid；
The extrusion molding of S3, hollow-fibre membrane：Using spinneret die, the composite braided pipe Jing Guo the pre-heat treatment is passed through into spray
Silk head applies simultaneously is covered with the spinning casting solution, and coagulating bath is entered after air section, is finally obtained in graphene/polyurethane
Empty fiber membrane；The composite braided pipe by the pre-heat treatment, which refers to, heats composite braided pipe, composite braided pipe
Temperature reaches 30~100 DEG C；
The leaching of S4, pore-foaming agent：Graphene prepared by step S3/polyurethane hollow fiber film immerses glycerin solution
In, the pore-foaming agent in film is removed, the temperature of glycerin solution is 25~30 DEG C, and soaking time is 4~8h；
S5, it dries：Graphene after immersion/polyurethane hollow fiber film is dried to get the graphene oxide/poly- ammonia
Ester hollow fiber ultrafiltration membrane.
Preferably, in step S1, vacuum drying temperature is 60~70 DEG C.
Preferably, the polyurethane is polyether polyurethane, and hardness is shore A90~95 degree；The graphene oxide is
After dissolution single layer content be 99% or more, flit size 0.5~2 μm, thickness 0.55~1.20nm graphene oxide.
Preferably, in step S3, the composite braided pipe refers to one in PET, PA, PE, PP, PES, PTFE and carbon fiber
Essentially continuous fine thread made of kind or several mixing materials.
Preferably, in step S3, refer to that by length be 2~5cm air section by air section.
Preferably, in step S3, the coagulating bath is carried out in the mixed liquor of water and solvent；The solvent is N,
The combination of one or more of dinethylformamide, n,N-dimethylacetamide, N-Methyl pyrrolidone, the mixed liquor
Middle solvent quality ratio is not higher than 50%.
Preferably, in step S4, the mass fraction of glycerine is 10~50% in the glycerin solution.
Preferably, it in step S5, dries and carries out at room temperature；And it is described under room temperature, air humidity is not
It obtains and is higher than 75%.
Compared with prior art, the beneficial effects of the present invention are：
1, polyurethane (PUR) material source is extensive, and cheap, manufacturing method is simple, is to replace to hold high after composite modified
The ideal membrane material of expensive Kynoar (PVDF)；
2, the coating that casting solution is formed firmly is attached to braiding pipe surface, and film wire flux is higher, toughness and impact resistance
Can be good, it is suitable for higher pressure backwash；
3, graphene obtained/polyurethane composite hollow fiber membrane has the function of catalysis, antibacterial etc., in sewage disposal process
In can play the role of accelerate pollutant oxidative degradation and prevent bacterium film surface breed, to improve the antipollution of film
Performance and wastewater treatment efficiency can provide high performance film product for MBR technique.
Detailed description of the invention
Upon reading the detailed description of non-limiting embodiments with reference to the following drawings, other feature of the invention,
Objects and advantages will become more apparent upon：
Fig. 1 is graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane cross-sectional scans Electronic Speculum schematic diagram, and outer layer is multiple
Filter membrane coating is closed, internal layer is that composite braided pipe makees supporting layer；
Fig. 2 is graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane surface scan Electronic Speculum schematic diagram；
Specific embodiment
The following describes the present invention in detail with reference to examples.Following embodiment will be helpful to those skilled in the art
The present invention is further understood, but the invention is not limited in any way.It should be pointed out that those skilled in the art
For, without departing from the inventive concept of the premise, it can also make certain adjustments and improvements.These belong to guarantor of the invention
Protect range.
Embodiment 1
PET and PA monofilament is woven into the composite braided pipe that homogeneous phase mutually interts with mass ratio for 49: 1, internal diameter is
2.0mm, wall thickness 0.2mm.Again by 35% polyurethane, 5% chliorinated polyvinyl chloride, 2% graphene oxide, 8% it is poly-
Ethylene glycol/polyvinylpyrrolidone (wt/wt=1/1), 4% Tween-80,46% dimethyl acetamide are agitated, and 90 DEG C
Under the conditions of dissolution 3h be configured to homogeneous casting solution；Spinning head is passed through after mixed weaving pipe is heated to 60 DEG C again, by 3cm air
Section, into containing 25%N, the coagulating bath of N- dimethyl acetamide.By casting solution after feed liquid pipeline introduces spinning head, material is opened
Liquid pipeline valve and establishment pipe are at the uniform velocity drawn.Then spinneret die is utilized, casting solution is coated uniformly on composite braided pipe surface,
Obtain graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane；Fig. 1 is graphene oxide obtained/polyurethane composite hollow
The cross-sectional scans Electronic Speculum schematic diagram of fiber ultrafiltration membrane, outer layer are composite filter membrane coating, and internal layer is that composite braided pipe makees supporting layer；Figure
2 be graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane surface scan Electronic Speculum schematic diagram, as shown in Figure 2, composite membrane table
Area-structure light cunning is smooth, has good self-cleaning function.
It obtains enhanced oxidation graphene/polyurethane composite hollow fibre ultrafiltration membrane and passes through performance test, be strongly much larger than
60N, pure water flux 1200LMH, initial bubble point 0.28MPa, film wire pass through 0.1MPa backwash air purge about 5min, film wire and branch
Support layer does not separate.In operating normally for common sanitary sewage disposal, influent COD (COD) is 500mg/
L, production water COD are 50mg/L, and COD removal rate is 90%.
Embodiment 2
PET and PTFE monofilament is woven into the composite braided pipe that homogeneous phase mutually interts with mass ratio for 40: 10, internal diameter is
2.0mm, wall thickness 0.2mm.Again by 38% polyurethane, 4% chliorinated polyvinyl chloride, 3% graphene oxide, 10% it is poly-
Ethylene glycol/polyvinylpyrrolidone (wt/wt=1/1), 5% Tween-80,40% dimethyl acetamide are agitated, and 90 DEG C
Under the conditions of dissolution 3h be configured to homogeneous casting solution；Spinning head is passed through after mixed weaving pipe is heated to 60 DEG C again, by 3cm air
Section, into containing 25%N, the coagulating bath of N- dimethyl acetamide.By casting solution after feed liquid pipeline introduces spinning head, material is opened
Liquid pipeline valve and establishment pipe are at the uniform velocity drawn.Then spinneret die is utilized, casting solution is coated uniformly on composite braided pipe surface,
Obtain graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane；
It obtains enhanced oxidation graphene/polyurethane composite hollow fibre ultrafiltration membrane and passes through performance test, be strongly much larger than
60N, pure water flux 1050LMH, initial bubble point 0.26MPa, film wire pass through 0.1MPa backwash air purge about 5min, film wire and branch
Support layer does not separate.In operating normally for common sanitary sewage disposal, influent COD (COD) is 500mg/
L, production water COD are 80mg/L, and COD removal rate is 84%.
Embodiment 3
PA and PES monofilament is woven into the composite braided pipe that homogeneous phase mutually interts with mass ratio for 50: 20, internal diameter is
2.0mm, wall thickness 0.2mm.Again by 45% polyurethane, 8% chliorinated polyvinyl chloride, 5% graphene oxide, 10% it is poly-
Ethylene glycol/polyvinylpyrrolidone (wt/wt=1/1), 5% Tween-80,27% dimethyl acetamide are agitated, and 90 DEG C
Under the conditions of dissolution 3h be configured to homogeneous casting solution；Spinning head is passed through after mixed weaving pipe is heated to 60 DEG C again, by 3cm air
Section, into containing 25%N, the coagulating bath of N- dimethyl acetamide.By casting solution after feed liquid pipeline introduces spinning head, material is opened
Liquid pipeline valve and establishment pipe are at the uniform velocity drawn.Then spinneret die is utilized, casting solution is coated uniformly on composite braided pipe surface,
Obtain graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane；
It obtains enhanced oxidation graphene/polyurethane composite hollow fibre ultrafiltration membrane and passes through performance test, be strongly much larger than
60N, pure water flux 950LMH, initial bubble point 0.29MPa, film wire pass through 0.1MPa backwash air purge about 5min, film wire and branch
Support layer does not separate.In operating normally for common sanitary sewage disposal, influent COD (COD) is 500mg/
L, production water COD are 60mg/L, and COD removal rate is 88%.
Embodiment 4
PA and PES monofilament is woven into the composite braided pipe that homogeneous phase mutually interts with mass ratio for 40: 20, internal diameter is
2.0mm, wall thickness 0.2mm.Again by 50% polyurethane, 6% chliorinated polyvinyl chloride, 3% graphene oxide, 8% it is poly-
Ethylene glycol/polyvinylpyrrolidone (wt/wt=1/1), 4% Tween-80,29% dimethyl acetamide are agitated, and 90 DEG C
Under the conditions of dissolution 3h be configured to homogeneous casting solution；Spinning head is passed through after mixed weaving pipe is heated to 60 DEG C again, by 3cm air
Section, into containing 25%N, the coagulating bath of N- dimethyl acetamide.By casting solution after feed liquid pipeline introduces spinning head, material is opened
Liquid pipeline valve and establishment pipe are at the uniform velocity drawn.Then spinneret die is utilized, casting solution is coated uniformly on composite braided pipe surface,
Obtain graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane；
It obtains enhanced oxidation graphene/polyurethane composite hollow fibre ultrafiltration membrane and passes through performance test, be strongly much larger than
60N, pure water flux 1100LMH, initial bubble point 0.27MPa, film wire pass through 0.1MPa backwash air purge about 5min, film wire and branch
Support layer does not separate.In operating normally for common sanitary sewage disposal, influent COD (COD) is 500mg/
L, production water COD are 80mg/L, and COD removal rate is 84%.
Embodiment 5
PA and PES monofilament is woven into the composite braided pipe that homogeneous phase mutually interts with mass ratio for 60: 10, internal diameter is
2.0mm, wall thickness 0.2mm.Again by 40% polyurethane, 8% chliorinated polyvinyl chloride, 2% graphene oxide, 9% it is poly-
Ethylene glycol/polyvinylpyrrolidone (wt/wt=1/1), 5% Tween-80,36% dimethyl acetamide are agitated, and 90 DEG C
Under the conditions of dissolution 3h be configured to homogeneous casting solution；Spinning head is passed through after mixed weaving pipe is heated to 60 DEG C again, by 3cm air
Section, into containing 25%N, the coagulating bath of N- dimethyl acetamide.By casting solution after feed liquid pipeline introduces spinning head, material is opened
Liquid pipeline valve and establishment pipe are at the uniform velocity drawn.Then spinneret die is utilized, casting solution is coated uniformly on composite braided pipe surface,
Obtain graphene oxide/polyurethane composite hollow fibre ultrafiltration membrane；
It obtains enhanced oxidation graphene/polyurethane composite hollow fibre ultrafiltration membrane and passes through performance test, be strongly much larger than
60N, pure water flux 1300LMH, initial bubble point 0.29MPa, film wire pass through 0.1MPa backwash air purge about 5min, film wire and branch
Support layer does not separate.In operating normally for common sanitary sewage disposal, influent COD (COD) is 500mg/
L, production water COD are 30mg/L, and COD removal rate is 94%.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (9)
1. a kind of graphene oxide/polyurethane hollow fiber ultrafiltration membrane, which is characterized in that its formula being film-made and its content are with matter
Percentages are measured, including：
The polyurethane weight average molecular weight is 350000, and the chliorinated polyvinyl chloride weight average molecular weight is 65000.
2. a kind of preparation method of graphene oxide as described in claim 1/polyurethane hollow fiber ultrafiltration membrane, feature exist
In described method includes following steps：
The pretreatment of S1, polymer material：Polyurethane, chliorinated polyvinyl chloride, graphene oxide are dried in vacuo at 60~80 DEG C
12~15h；
The preparation of S2, casting solution：In proportion by polyurethane, chliorinated polyvinyl chloride, graphene oxide, pore-foaming agent, hydrophilic agent, solvent
After weighing mixing, 80~100 DEG C at a temperature of be stirred dissolution, mixing time is 15~for 24 hours, speed of agitator for 80~
120 revs/min, after acquired solution vacuumizing and defoaming, 1h or more is stood, spinning casting solution is obtained；
The extrusion molding of S3, hollow-fibre membrane：Using spinneret die, the composite braided pipe Jing Guo the pre-heat treatment is passed through into spinning head
It applies simultaneously and is covered with the spinning casting solution, coagulating bath is entered after air section, finally obtains the hollow fibre of graphene/polyurethane
Tie up film；The composite braided pipe by the pre-heat treatment, which refers to, heats composite braided pipe, composite braided tube temperature degree
Reach 30~100 DEG C；
The leaching of S4, pore-foaming agent：Graphene prepared by step S3/polyurethane hollow fiber film immerses in glycerin solution,
The pore-foaming agent in film is removed, the temperature of glycerin solution is 25~30 DEG C, and soaking time is 4~8h；
S5, it dries：Graphene after immersion/polyurethane hollow fiber film is dried to get in the graphene oxide/polyurethane
Fibre ultrafiltration film.
3. preparation method according to claim 2, which is characterized in that in step S1, vacuum drying temperature is 60~70
℃。
4. preparation method according to claim 2, which is characterized in that the polyurethane is polyether polyurethane, and hardness is
Shore A90~95 degree；The graphene oxide is that single layer content is 99% or more, flit size is in 0.5~2 μm, thickness after dissolving
Spend the graphene oxide in 0.55~1.20nm.
5. preparation method according to claim 2, which is characterized in that in step S3, the composite braided pipe refer to PET,
Essentially continuous fine thread made of one or more of PA, PE, PP, PES, PTFE and carbon fiber mixing material.
6. preparation method according to claim 2, which is characterized in that in step S3, refer to by air section by length
For 2~5cm air section.
7. preparation method according to claim 2, which is characterized in that in step S3, the coagulating bath be with water with it is molten
It is carried out in the mixed liquor of agent；The solvent is n,N-Dimethylformamide, n,N-dimethylacetamide, N-Methyl pyrrolidone
One or more of combination, solvent quality ratio is not higher than 50% in the mixed liquor.
8. preparation method according to claim 2, which is characterized in that in step S4, the third three in the glycerin solution
The mass fraction of alcohol is 10~50%.
9. preparation method according to claim 2, which is characterized in that in step S5, drying is to carry out at room temperature
's；And it is described under room temperature, air humidity must not be higher than 75%.
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| Publication number | Publication date |
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| CN108854600B (en) | 2021-07-30 |
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