CN106621833A - Preparation method of ultrafiltration membrane with anti-fouling performance enhanced by nitrogen-doped graphene oxide/TiO2 composite particles - Google Patents
Preparation method of ultrafiltration membrane with anti-fouling performance enhanced by nitrogen-doped graphene oxide/TiO2 composite particles Download PDFInfo
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- CN106621833A CN106621833A CN201611179911.0A CN201611179911A CN106621833A CN 106621833 A CN106621833 A CN 106621833A CN 201611179911 A CN201611179911 A CN 201611179911A CN 106621833 A CN106621833 A CN 106621833A
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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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Abstract
The invention discloses a preparation method of an ultrafiltration membrane with anti-fouling performance enhanced by nitrogen-doped graphene oxide/TiO2 composite particles. The preparation method comprises the following steps: (1) preparing the nitrogen-doped graphene oxide / TiO2 composite particles; (2) adding an organic solvent in the nitrogen-doped graphene oxide / TiO2 composite particles, uniformly dispersing, then adding a membrane material and a membrane additive, and mixing evenly to obtain a casting membrane solution; and (3) after defoaming of the casting membrane solution stops, pouring the casting membrane solution on the surface of a clean and smooth flat plate, stably and rapidly scraping the casting membrane solution by using a membrane blade, and placing the casting membrane solution in a gel phase to obtain the ultrafiltration membrane. The polysulfone ultrafiltration membrane with high hydrophilicity and anti-fouling performance is prepared by phase inversion, a water contact angle of the prepared polysulfone ultrafiltration membrane is reduced obviously, and is reduced to be about 61 degrees from about 88 degrees, and therefore, the anti-fouling ability of the membrane is improved.
Description
Technical field
The present invention relates to a kind of preparation method of milipore filter, more particularly, to a kind of nitrating graphene oxide/TiO is utilized2
Composite particles strengthen the preparation method of the milipore filter of resistance tocrocking.
Background technology
Ultrafiltration is a kind of membrane separating process, is colloid, bulky grain and molecular weight phase in trap water under ambient pressure effect
To higher material, and water and little particles of solute pass through the separation process of film.Because hyperfiltration technique has normal-temperature operation, process
Without it is covert, energy consumption is low, separative efficiency is high the advantages of, drink water purifying, petrochemical industry, bio-pharmaceuticals, video, metallurgy etc. again at present
Industry is widely applied.
PS membrane has strong oxidative resistance, and with cheap and easy to get, good mechanical strength, the close property of resistance to compression and chemically stable
Property, heat resistance and the advantages of wide pH value use ranges, but its hydrophobicity is also that people all knows, the main performance of its harm
Easily absorption is produced in hydrophobic solutes on film surface and deposited, cause fouling membrane, reduce the performance and the service life for shortening film of film.
Therefore, PS membrane is carried out hydrophilically modified, improves its contamination resistance very necessary.
At present, hydrophilically modified method is carried out to milipore filter mainly modified surface, blending and modifying and chemical modification etc..
Relative to other two kinds of method of modifying, blending and modifying has operation relatively easy, and modified effect is good, the advantages of economical and practical.Have
Machine-inorganic blending operations are simple, excellent performance, add hydrophilic inorganic nano particle to increase film surface hydrophilicity, reduce film
Pollution, while improve film mechanical performance, be study hotspot in recent years.
TiO2Particle contains nano-TiO due to ultrahydrophilic, extremely strong photocatalytic and the function such as nontoxic, preparation2Have
Machine-inorganic hybridization membrane material has caused the extensive concern of researcher with the mutual supplement with each other's advantages for realizing both.But TiO2With easily reunion
The shortcoming of property, have impact on its extensive application in field of membrane material.Nitrating graphene oxide, as the derivative of Graphene, tool
There are the properties such as good electric conductivity, hydrophily, heat endurance and mechanical strength, it is used as TiO2Carrier can greatly improve
The dispersiveness of titanium dioxide and hydrophily.
The content of the invention
The technical problem to be solved is the defect for overcoming prior art, there is provided one kind utilizes nitrating graphite oxide
Alkene/TiO2Composite particles strengthen the preparation method of the milipore filter of resistance tocrocking.The present invention is prepared using phase inversion has high parent
The polysulphone super-filter membrane of aqueous and resistance tocrocking, the water contact angle of made polysulphone super-filter membrane is substantially reduced, is reduced to from 88 ° or so
61 ° or so, improve the contamination resistance of film.
To solve above-mentioned technical problem, the present invention provides a kind of using nitrating graphene oxide/TiO2Composite particles strengthen
The preparation method of the milipore filter of resistance tocrocking, is characterized in that, comprise the following steps:
(1)Nitrogen oxidation Graphene/TiO2The preparation of composite particles
Weigh graphene oxide to be placed in beaker, with distillation water dissolves, ultrasonic vibration 1h makes graphene oxide be uniformly dispersed;Claim
Take urea to be dissolved into graphene oxide solution, stir;The solution for preparing is put into reactor and is heated, obtain black
Solution;Dark solution is added and obtain nitrating graphene oxide particle after distilled water cyclic washing and freeze-drying;By nitrating oxygen
Graphite alkene and TiO2Particle is placed in beaker and dissolves, and after ultrasonic vibration 30min, is put into reactor and heats, and obtains grey molten
Liquid;Grey solution is added and obtain nitrating graphene oxide/TiO after distilled water cyclic washing and freeze-drying2Composite particles;
(2)Nitrating graphene oxide/TiO2After adding organic solvent, decentralized processing uniform in composite particles, addition membrane material,
Film additive, obtains casting solution after being well mixed;
(3)After by casting solution discontinuous degassing, clean smooth planar surface is poured over, after steadily being scraped rapidly with knifing machine, is put
In entering gel phase, milipore filter is obtained.The gel is mutually using water, water and solvent mixed liquor, water and absolute ethyl alcohol mixed liquor, air
In one kind, wherein, solvent mixed liquor be 1-METHYLPYRROLIDONE, N-N- dimethylformamides, N-N- dimethyl acetamides in
A kind of constituted mixed liquor;To gel mutually this process elapsed time referred to as dry journey is put into after knifing, do
The length of journey can have a strong impact on the pore-size distribution on prepared film surface, therefore it is preferred that the dry journey is 0~2min.
Further, above-mentioned steps(1)In, the graphene oxide is 1 with the mass ratio of urea:4.
Further, above-mentioned steps(1)In, answer heating condition in kettle to be to heat 24 hours at 180 DEG C described.
Further, above-mentioned steps(1)In, the nitrating graphene oxide and TiO2The mass ratio of particle is 7:3.
Further, the TiO2Particle is prepared by sol-gal process, and concrete operation method is as follows:
Solution A:By butyl titanate and absolute ethyl alcohol by volume 1:4 are well mixed in beaker;
B solution:By absolute ethyl alcohol, pure water, glacial acetic acid by volume 5:2:1 prepares mixed solution, and adjusts PH=2 with watery hydrochloric acid,
B solution is dropwise added drop-wise in solution A, and persistently stirs 30min, it is stirred after, by the static 3h gels of mixed solution;
Above-mentioned spawn is placed in air dry oven 24h is dried at 100 DEG C, powdery is ground to form after cooling, then be placed in
500 DEG C of calcining 2h are heated to the speed of 2 DEG C/min in resistance furnace, are taken out after natural cooling and is obtained TiO2Particle.
Further, above-mentioned steps(2)In, the nitrating graphene oxide/TiO2The addition content of composite particles is
0.1~0.8%, content refers to the mass fraction relative to casting solution.Nitrating graphene oxide/TiO2The addition of composite particles
The performance tool of milipore filter is had a significant impact, because nitrating graphene oxide/TiO2Composite particles add membership to affect split-phase mistake
Journey, so as to affect the aperture of film, with nitrating graphene oxide/TiO2The increase of composite particles addition, the aperture of milipore filter
First increases and then decreases.
Further, above-mentioned steps(2)In, the organic solvent be 1-METHYLPYRROLIDONE, N-N- dimethylformamides,
One kind in N-N- dimethyl acetamides, organic solvent content is 75~90%, and content refers to the quality point relative to casting solution
Number.
Further, above-mentioned steps(2)In, described film additive is polyvinyl pyrrolidone, polyethylene glycol, poly- second
One kind in enol, the content of film additive is 0~4%, and content refers to the mass fraction relative to casting solution.
Further, above-mentioned steps(2)In, described decentralized processing is processed using ultrasonication, stir process, concussion
In one kind.Nitrating graphene oxide/TiO can be made2Composite particles are uniformly dispersed in organic solvent again, and preferably described divides
The scattered time is 2h.
Further, above-mentioned steps(2)In, described membrane material is polysulfones, and the content of membrane material is 16~25%, content
Refer to the mass fraction relative to casting solution.
The beneficial effect that the present invention is reached:
(1)Nitrating graphene oxide/TiO2Composite particles can uniformly, be well dispersed into solvent or casting solution, this is very big
Improve nitrating graphene oxide/TiO2Contact and compatibility of the composite particles with film, is more beneficial for playing its own feature;
(2)Nitrating graphene oxide/TiO2The addition of composite particles makes the water contact angle of milipore filter substantially reduce, from 88 ° or so
61 ° or so are reduced to, the antifouling property of film is improve;
(3)Nitrating graphene oxide/the TiO of the present invention2Composite particles preparation method is simple, it is easy to industrialized production application.
Description of the drawings
Fig. 1 is embodiment 1~4 with ultrafiltration membrane surface water contact angle in comparative example with nitrating graphene oxide/TiO2It is compound
The change of granule content;
Fig. 2 is embodiment 1~4 with ultrafiltration membrane surface protein adsorption quantity in comparative example with nitrating graphene oxide/TiO2Compound
The change of grain content.
Specific embodiment
Below in conjunction with the accompanying drawings the invention will be further described.Following examples are only used for clearly illustrating the present invention
Technical scheme, and can not be limited the scope of the invention with this.
Embodiment 1
Present embodiments provide a kind of containing 0.1% nitrating graphene oxide/TiO2The preparation method of composite particles polysulphone super-filter membrane,
Comprise the following steps that:
(1)350mg graphene oxides are placed in beaker, add 90mL deionized waters, ultrasonic vibration 1h uniformly to be aoxidized
Graphene solution.1.2g urea is added toward graphene oxide solution, and persistently stirs 1h and obtain uniform mixed solution.Will be mixed
Conjunction solution is put into 150mL reactors and heats 24h at 180 DEG C.Question response kettle is naturally cooled to after room temperature, by the black for obtaining
Solid deionized water is rinsed 3 times repeatedly, and nitrating graphene oxide is obtained after freeze-drying;
(2)Solution A:To be well mixed in 10mL butyl titanates and 40mL absolute ethyl alcohol beakers.B solution:By absolute ethyl alcohol, pure
Water, glacial acetic acid take respectively 10mL, 4mL, 2mL and are well mixed, and adjust PH=2 with watery hydrochloric acid.B solution is dropwise added drop-wise to solution A
In, and persistently stir 30min.After stirred, by the static 3h gels of mixed solution.Above-mentioned spawn is placed in into air blast
24h is dried at 100 DEG C in drying box, powdery is ground to form after cooling, then be placed in resistance furnace and be heated to the speed of 2 DEG C/min
500 DEG C of calcining 2h, take out after natural cooling and obtain TiO2Particle;
(3)Take 350mg nitratings graphene oxide and 210mg TiO2In being placed in beaker, 100mL water is added to obtain under ultrasound condition
To uniform mixed liquor.Mixed solution is put into 150mL reactors and heats 24h at 180 DEG C.Question response kettle naturally cools to room
Wen Hou, the gray solid deionized water for obtaining is rinsed 3 times repeatedly, and nitrating graphene oxide/TiO is obtained after freeze-drying2
Composite particles;
(4)By 100mg nitratings graphene oxide/TiO2Composite particles are scattered in 78.9gN- crassitudes under ultrasound condition
Ketone(NMP)In, after ultrasonic 2h, PVP 3g, polysulfones 18g are added to the solution under stirring, stir at 50 DEG C
6h is mixed, uniform casting solution is formed;
(5)By the static 24h deaerations of casting solution.After deaeration, at ambient temperature, using knifing by casting solution on a glass
Machine(Its scraper is 100 μm)Film is uniformly scraped on a glass, and is immediately moved into coagulation bath(Water)After 1~2min visible film from
It is dynamic to depart from glass plate;24h is soaked in deionized water, it is ensured that phase transfer completely;Film is placed between two layers of filter paper, greenhouse wind
Dry, preparation is completed.
Containing 0.1% nitrating graphene oxide/TiO2Experiment is investigated in the protein absorption of composite particles modified polysulfone film, specifically
Operation is as follows:
The milipore filter that one prepares is cut into the diaphragm of diameter 2.5cm, the bovine serum albumen solution containing 500mg/L is entered
In, under the rotating speed of 100r/min, adsorb 24h, by determined by ultraviolet spectrophotometry solution remain protein content, so as to
The amount of absorption is drawn, experimental result is shown in Fig. 2.
Figure it is seen that containing 0.1% nitrating graphene oxide/TiO2The protein 24h of the PS membrane of composite particles inhales
Attached amount is relatively low, with good protein contamination.
Embodiment 2~4
Only change nitrating graphene oxide/TiO2The content of composite particles is 0.3%, 0.5% and 0.8%, other same embodiments of operation
1, gained nitrating graphene oxide/TiO2The modified PS membrane of composite particles has different antipollution effects, sees Fig. 2.
Embodiment 5~6
Organic solvent in embodiment 1 is changed the one kind made in N-N- dimethylformamides, N-N- dimethyl acetamides, other behaviour
Make with embodiment 1, gained nitrating graphene oxide/TiO2The antipollution effect and embodiment 1 of the modified PS membrane of composite particles
It is essentially identical.
Embodiment 7~8
One kind that film additive in embodiment 1 is changed in making polyethylene glycol, polyvinyl alcohol, other operations are with embodiment 1, gained
Nitrating graphene oxide/TiO2The antipollution effect of the modified PS membrane of composite particles is substantially the same manner as Example 1.
Comparative example 1
It is added without nitrating graphene oxide/TiO2To in PS membrane, other operations are with embodiment 1, gained PS membrane for composite particles
Resistance tocrocking is poor, sees Fig. 2.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, on the premise of without departing from the technology of the present invention principle, some improvement and deformation can also be made, these improve and deform
Also should be regarded as protection scope of the present invention.
Claims (10)
1. it is a kind of to utilize nitrating graphene oxide/TiO2Composite particles strengthen the preparation method of the milipore filter of resistance tocrocking, and it is special
Levying is, comprises the following steps:
(1)Nitrogen oxidation Graphene/TiO2The preparation of composite particles
Weigh graphene oxide to be placed in beaker, with distillation water dissolves, ultrasonic vibration 1h makes graphene oxide be uniformly dispersed;Claim
Take urea to be dissolved into graphene oxide solution, stir;The solution for preparing is put into reactor and is heated, obtain black
Solution;Dark solution is added and obtain nitrating graphene oxide particle after distilled water cyclic washing and freeze-drying;By nitrating oxygen
Graphite alkene and TiO2Particle is placed in beaker and dissolves, and after ultrasonic vibration 30min, is put into reactor and heats, and obtains grey molten
Liquid;Grey solution is added and obtain nitrating graphene oxide/TiO after distilled water cyclic washing and freeze-drying2Composite particles;
(2)Nitrating graphene oxide/TiO2After adding organic solvent, decentralized processing uniform in composite particles, membrane material, film are added
Additive, obtains casting solution after being well mixed;
(3)After by casting solution discontinuous degassing, clean smooth planar surface is poured over, after steadily being scraped rapidly with knifing machine, is put
In entering gel phase, milipore filter is obtained.
2. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(1)In, the graphene oxide is 1 with the mass ratio of urea:4.
3. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(1)In, answer heating condition in kettle to be that heating 24 is little at 180 DEG C described
When.
4. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(1)In, the nitrating graphene oxide and TiO2The mass ratio of particle is
7:3.
5. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, the TiO2Particle is prepared by sol-gal process, and concrete operation method is as follows:
Solution A:By butyl titanate and absolute ethyl alcohol by volume 1:4 are well mixed in beaker;
B solution:By absolute ethyl alcohol, pure water, glacial acetic acid by volume 5:2:1 prepares mixed solution, and adjusts PH=2 with watery hydrochloric acid,
B solution is dropwise added drop-wise in solution A, and persistently stirs 30min, it is stirred after, by the static 3h gels of mixed solution;
Above-mentioned spawn is placed in air dry oven 24h is dried at 100 DEG C, powdery is ground to form after cooling, then be placed in
500 DEG C of calcining 2h are heated to the speed of 2 DEG C/min in resistance furnace, are taken out after natural cooling and is obtained TiO2Particle.
6. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(2)In, the nitrating graphene oxide/TiO2The addition of composite particles
Content is 0.1~0.8%, and content refers to the mass fraction relative to casting solution.
7. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(2)In, the organic solvent is 1-METHYLPYRROLIDONE, N-N- dimethyl
One kind in formamide, N-N- dimethyl acetamides, organic solvent content is 75~90%, and content is referred to relative to casting solution
Mass fraction.
8. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(2)In, described film additive is polyvinyl pyrrolidone, poly- second two
One kind in alcohol, polyvinyl alcohol, the content of film additive is 0~4%, and content refers to the mass fraction relative to casting solution.
9. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(2)In, described decentralized processing using ultrasonication, stir process,
One kind in concussion process, described jitter time is 2h.
10. according to claim 1 a kind of using nitrating graphene oxide/TiO2Composite particles strengthen the super of resistance tocrocking
The preparation method of filter membrane, is characterized in that, above-mentioned steps(2)In, described membrane material is polysulfones, the content of membrane material is 16~
25%, content refers to the mass fraction relative to casting solution.
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CN107552082A (en) * | 2017-09-29 | 2018-01-09 | 河海大学 | A kind of quaternary multifunction magnetic nano composite material and preparation method thereof |
CN108176232A (en) * | 2017-12-30 | 2018-06-19 | 孙祎 | A kind of preparation method of the charged membrane material of pollution-resistant |
CN108479424A (en) * | 2018-04-02 | 2018-09-04 | 合肥国轩高科动力能源有限公司 | Preparation method of modified polyvinylidene fluoride membrane |
CN108927225A (en) * | 2018-06-27 | 2018-12-04 | 浙江工业大学膜分离与水处理协同创新中心湖州研究院 | A kind of photocatalysis membrana preparation method for dyestuff degradation |
CN109453679A (en) * | 2018-10-30 | 2019-03-12 | 江苏理工学院 | A kind of preparation method of nitrating graphene oxide titanium dioxide composite hyperfiltration membrane |
CN111715079A (en) * | 2020-05-20 | 2020-09-29 | 嘉兴市轩禾园艺技术有限公司 | Multifunctional film material and preparation method and application thereof |
CN111760461A (en) * | 2020-06-24 | 2020-10-13 | 上海应用技术大学 | Preparation method of polyvinylidene fluoride mixed matrix film |
CN112774464A (en) * | 2020-12-17 | 2021-05-11 | 中国科学院过程工程研究所 | Forward osmosis composite membrane and preparation method and application thereof |
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CN109453679A (en) * | 2018-10-30 | 2019-03-12 | 江苏理工学院 | A kind of preparation method of nitrating graphene oxide titanium dioxide composite hyperfiltration membrane |
CN111715079A (en) * | 2020-05-20 | 2020-09-29 | 嘉兴市轩禾园艺技术有限公司 | Multifunctional film material and preparation method and application thereof |
CN111760461A (en) * | 2020-06-24 | 2020-10-13 | 上海应用技术大学 | Preparation method of polyvinylidene fluoride mixed matrix film |
CN111760461B (en) * | 2020-06-24 | 2022-08-23 | 上海应用技术大学 | Preparation method of polyvinylidene fluoride mixed matrix membrane |
CN112774464A (en) * | 2020-12-17 | 2021-05-11 | 中国科学院过程工程研究所 | Forward osmosis composite membrane and preparation method and application thereof |
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