CN109675442A - A kind of preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film - Google Patents
A kind of preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film Download PDFInfo
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- CN109675442A CN109675442A CN201910025358.2A CN201910025358A CN109675442A CN 109675442 A CN109675442 A CN 109675442A CN 201910025358 A CN201910025358 A CN 201910025358A CN 109675442 A CN109675442 A CN 109675442A
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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
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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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
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0044—Inorganic membrane manufacture by chemical reaction
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- B01D2325/36—Hydrophilic membranes
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to environment functional material technical fields, and in particular to a kind of preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film；Specific steps are as follows: firstly, dispersing n,N-Dimethylformamide in isopropanol, four tincture ester of metatitanic acid is added, after stirring, cobalt chloride hexahydrate is added, obtains mixed liquor after stirring；Carbon cloth is immersed into mixed liquor again, then, mixed liquor is moved to and carries out heating reaction in ptfe autoclave, after reaction cooled to room temperature, super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film is obtained after cleaned, dry；Super hydrophilic/underwater superoleophobic visible optical drive pollution resistance UF membrane produced by the present invention is high-efficient, and separative efficiency is up to 99% or more；And performance is stable, pollution resistance is strong, also has excellent regenerability.
Description
Technical field
The invention belongs to environment functional material technical fields, and in particular to a kind of super hydrophilic/underwater superoleophobic visible CD-ROM drive
The preparation method of dynamic pollution resistance film.
Background technique
As frequent oil spill events constantly occur and the continuous discharge of oil-containing industrial water, have resulted in serious
Ecocrisis.A large amount of oily wastewaters enter water environment, not only the valuable water resource of serious pollution, cause huge economic damage
It loses, influences the development of society.So a kind of method for finding effective processing oily waste water has become a top priority.Traditional
Oil-water separation method has bioanalysis, absorption method and supercritical ultrasonics technology, but since its low separation efficiency, operating difficulties, separation process are multiple
It is miscellaneous, cause the effect of oil-water separation mixture not ideal enough.Therefore, a kind of method of simply and effectively processing oily waste water is developed
It seems very necessary.
In recent years, the development of special wetability material provides an effective way for water-oil separating.By constructing micro-nano
Rice composite construction and low-surface-energy material, have continuously synthesized a large amount of artificial super-hydrophobic film.However, these super hydrophobic materials due to
It is not suitable for separating the oil water mixture of rich water with lipophilicity, easily causing hole plug and hydrophobicity reduces, to reduce
The service life of membrane material；Currently, be developed rapidly in terms of Oil-water separation in super hydrophilic/underwater super hydrophobic material, it is existing
There is literature research to report modified pvdf membrane, sponge, the stainless steel nethike embrane etc. of hydroaropic substance, these materials allow water to pass through,
The oil in film surface can be repelled simultaneously, be polluted by the oil to effectively prevent film；But there are still many deficiencies, due in oil
During water separation, film surface is still attached with a small amount of oil, causes separative efficiency to reduce, flux is reduced.Therefore, one kind is prepared
Membrane material with excellent antifouling property is of great significance for water-oil separating.
Summary of the invention
Aiming at the shortcomings in the prior art, present invention seek to address that one of described problem；The present invention provides a kind of super close
Water/underwater superoleophobic visible optical drive pollution resistance film preparation method, the TiO for being adulterated Co by a step solvent-thermal method2Load
Super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film is obtained on carbon cloth, after drying, and there is high separative efficiency, it is excellent
Antifouling property and good power of regeneration.
In order to achieve the goal above, the specific steps of the present invention are as follows:
(1) firstly, dispersing n,N-Dimethylformamide (DMF) in isopropanol (IPA), four tincture ester of metatitanic acid is added, stirs
After mixing, cobalt chloride hexahydrate (CoCl is added2·6H2O it) stirs, obtains mixed liquor；
(2) in the mixed liquor for obtaining carbon cloth immersion step (1), then, mixed liquor is moved into ptfe autoclave
In carry out heating reaction, cooled to room temperature after reaction, obtained after cleaned, dry it is super hydrophilic/underwater it is superoleophobic can
Light-exposed driving pollution resistance film.
Preferably, n,N-Dimethylformamide described in step (1), isopropanol, four tincture ester of metatitanic acid and cobalt chloride hexahydrate
Amount ratio be 10~30mL:20~40mL:1~3mL:16~48mg.
Preferably, mixing time described in step (1) is 15min.
Preferably, temperature described in step (2) is 180~220 DEG C, and the time is 18~22h.
Preferably, cleaning described in step (2) is rinsed well with deionized water.
Preferably, temperature dry described in step (2) be 60 DEG C, time 6h.
Superoleophobic visible optical drive pollution resistance film super hydrophilic obtained by the present invention/underwater has super hydrophilic/underwater super thin
Oily characteristic, separative efficiency is high, and performance is stablized, and anti-pollution and regeneration performance are good, can be applied to environmental wastewater processing.
The beneficial effects of the present invention are:
(1) contact angle is 0 °, water in super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film air produced by the present invention
Lower oil contact angle is greater than 150 °, it can thus be seen that the film has super hydrophilic/underwater superoleophobic characteristic；Simultaneously in carbon cloth surfaces
The TiO of close attachment Co doping2Three-dimensional net structure in nanosphere, with carbon cloth forms micro-nano multilevel structure, is conducive to material
The superoleophobic property of material.
(2) super hydrophilic/underwater superoleophobic visible optical drive pollution resistance UF membrane produced by the present invention is high-efficient, to different oil
The separative efficiency of aqueous mixtures is up to 99% or more；
(3) super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film properties prepared by the present invention are stable, pollution resistance is strong,
It under visible optical drive, is recycled by 110 water-oil separating, super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film is still
Keep higher separative efficiency, show super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film it is with good stability and
Pollution resistance；
(4) super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared by the present invention has excellent regenerability,
After 110 water-oil separating, under super hydrophilic/underwater superoleophobic visible optical drive pollution resistance membrane separation efficiency does not have substantially
Drop illustrates that super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film has excellent power of regeneration；
(5) persursor material used in the present invention is carbon cloth, and electric conductivity is good；Moreover, operation of the present invention process operates
It is simple and easy, do not need Large expensive instrument, be economic and environment-friendly.
Detailed description of the invention
(a) is that the SEM of 500 times of original carbon cloth schemes in Fig. 1；(b) scheme for the SEM of 3000 times of original carbon cloth.
(a) is prepared super hydrophilic/superoleophobic visible 10000 times of optical drive pollution resistance film underwater in Fig. 2 for embodiment 2
SEM figure；(b) super hydrophilic/underwater superoleophobic visible 50000 times of optical drive pollution resistance film of the SEM figure prepared for embodiment 2
(a) is that water connects in super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film air of the preparation of embodiment 2 in Fig. 3
Feeler figure；(b) oily contact angle figure in super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film water prepared for embodiment 2；
(c) super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared for embodiment 2 oil droplet figure in water.
Fig. 4 is the experimentation of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared by embodiment 2, wherein
(a) it is the picture before petroleum ether-aqueous mixtures separation, is (b) picture after petroleum ether-aqueous mixtures separation, (c) is dichloro
Picture before methane-aqueous mixtures separate is (d) picture after methylene chloride-aqueous mixtures separation.
Fig. 5 is super hydrophilic/underwater superoleophobic visible optical drive pollution resistance UF membrane difference oil mixing with water prepared by embodiment 2
The separative efficiency and water flux of object.
(2) are super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of the preparation of embodiment 2 by diesel oil dirt in Fig. 6
After dye after radiation of visible light aerial water contact angle figure；It (b) can for the super hydrophilic/superoleophobic under water of the preparation of embodiment 2
Light-exposed driving pollution resistance film oily contact angle figure under water after radiation of visible light after by contaminated by diesel oil.
Fig. 7 is 110 water-oil separating before super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared by embodiment 2
Underwater oily contact angle.
Specific embodiment
In order to clarify the technical solutions and technical objectives of the present invention, with reference to the accompanying drawing and specific embodiment is the present invention
It is further to introduce.
Embodiment 1:
(1) stir 15min firstly, dispersing the n,N-Dimethylformamide of 20mL in the isopropanol of 20mL, then plus
Enter four tincture ester of 1mL metatitanic acid, stirs 15min, add the cobalt chloride hexahydrate of 16mg, obtain mixed liquor；
(2) mixed solution being moved in ptfe autoclave, carbon cloth is added, the area of carbon cloth is 2.5cm x3cm,
Heating reaction, temperature is 180 DEG C, time 18h, after room temperature, takes out carbon cloth compound, is rinsed with deionized water
Completely, in an oven 60 DEG C of dry 12h to get to super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film.
Embodiment 2:
(1) stir 15min firstly, dispersing the n,N-Dimethylformamide of 10mL in the isopropanol of 30mL, then plus
Enter four tincture ester of 2mL metatitanic acid, stirs 15min, add the cobalt chloride hexahydrate of 32mg, obtain mixed liquor；
(2) mixed solution being moved in ptfe autoclave, carbon cloth is added, the area of carbon cloth is 2.5cm x3cm,
Heating reaction, temperature is 200 DEG C, time 20h, after room temperature, takes out carbon cloth compound, is rinsed with deionized water
Completely, in an oven 60 DEG C of dry 12h to get to super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film.
Embodiment 3:
(1) stir 15min firstly, dispersing the n,N-Dimethylformamide of 30mL in the isopropanol of 40mL, then plus
Enter four tincture ester of 3mL metatitanic acid, stirs 15min, add the cobalt chloride hexahydrate of 48mg, obtain mixed liquor；
(2) mixed solution being moved in ptfe autoclave, carbon cloth is added, the area of carbon cloth is 2.5cm x3cm,
Heating reaction, temperature is 220 DEG C, time 22h, after room temperature, takes out carbon cloth compound, is rinsed with deionized water
Completely, in an oven 60 DEG C of dry 12h to get to super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film.
2, below with reference to specific implementation example, the present invention will be further described:
Separating property evaluation carries out by the following method in specific embodiment in the present invention: firstly, the film that will be prepared
Material is fixed between two quartz tube devices as filter membrane, and a small beaker is placed below for collecting water in filter.
Then, oil water mixture (V is preparedOil:VWater=1:1) it is used as oily waste water.Finally, oily waste water is poured on film, separation is weighed
The amount of water after preceding and separation.Select hexane and methylene chloride for representative in the present embodiment.Separative efficiency (η) is by following equation meter
It calculates:
Wherein m0(g) and m1(g) be respectively water primary quantity and time t in penetrate the quality of film.
Fluid flux is calculated by following formula:
Wherein J (Lm-2·h-1) it is fluid flux, V (L) is the permeation volume of water, S (m2) be film effective contact surface
Product, △ t (h) are time of penetration.
(a) is that the SEM of 500 times of original carbon cloth schemes in Fig. 1；(b) scheme for the SEM of 3000 times of original carbon cloth；It can from Fig. 1
To find out that original carbon cloth has three-dimensional structure, smooth fiber interweaving together, is conducive to the negative of inorganic nano-particle in carbon cloth
It carries.
In figure 2 (a) be prepared for embodiment 2 it is superoleophobic visible 10000 times of optical drive pollution resistance film super hydrophilic/underwater
SEM figure；(b) super hydrophilic/underwater superoleophobic visible 50000 times of optical drive pollution resistance film of the SEM figure prepared for embodiment 2；
From figure (a) it can be seen that the three-dimensional net structure film film of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film loads one layer
The TiO of fine and close Co doping2Nanosphere；From in (b) it can be seen that super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film
Surface has the nanosphere of one layer of amplification factor, forms micro-nano multilevel structure with three-dimensional net structure, is conducive to improve material
Coarse structure, to facilitate reinforcing material superoleophobic property under water.
(a) is that water connects in super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film air of the preparation of embodiment 2 in Fig. 3
Feeler figure；(b) oily contact angle figure in super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film water prepared for embodiment 2；
(c) super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared for embodiment 2 oil droplet figure in water.It can be with from figure (a)
The water contact angle for seeing super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film is 0 °, is Superhydrophilic；It can be with from figure (b)
The underwater oily contact angle for seeing super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film is 157 ° ± 1 ° (150 ° of >), performance
Superoleophobic property under water outlet；Can see from figure (c) can be steady in super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film oil droplet
Exist calmly and be approximately spherical shape, it is underwater super to further demonstrate that super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film has
Oleophobic property.
Fig. 4 is the experimentation of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared by embodiment 2, wherein
(a) it is the picture before petroleum ether-aqueous mixtures separation, is (b) picture after petroleum ether-aqueous mixtures separation, (c) is dichloro
Picture before methane-aqueous mixtures separate is (d) picture after methylene chloride-aqueous mixtures separation.Show super hydrophilic/underwater super
The visible optical drive pollution resistance film of oleophobic can not only separate light oil can also be with heavy oil separation.
Fig. 5 is super hydrophilic/underwater superoleophobic visible optical drive pollution resistance UF membrane difference oil mixing with water prepared by embodiment 2
The separative efficiency and water flux of object；This demonstrate super hydrophilic/underwater superoleophobic visible optical drive pollution resistance films can separate light/weight
Oil-aqueous mixtures, and there is high separative efficiency to be higher than 99% various oil water mixtures, and for toluene, hexamethylene, stone
The grease flux that oily ether, hexane class density are less than water is above 24000L m-2h-1, for diesel oil, soybean oil, dichloromethane alkanes
Viscous oil water flux also above 18300L m-2h-1, show high separative efficiency and flux.
(2) are super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of the preparation of embodiment 2 by diesel oil dirt in Fig. 6
After dye after radiation of visible light aerial water contact angle figure；It (b) can for the super hydrophilic/superoleophobic under water of the preparation of embodiment 2
Light-exposed driving pollution resistance film oily contact angle figure under water after radiation of visible light after by contaminated by diesel oil.As can be seen from Figure,
Super hydrophilic/underwater superoleophobic characteristic is lost by the film of contaminated by diesel oil, when by restored after radiation of visible light it is super hydrophilic/
Underwater superoleophobic property shows that super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film has excellent pollution resistance.
Fig. 7 is 110 water-oil separating before super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film prepared by embodiment 2
Underwater oily contact angle.Under can be seen that super hydrophilic/20-30 contact angle of underwater superoleophobic visible optical drive pollution resistance film gradually
Drop loses superoleophobic property super hydrophilic in air/underwater.When having restored underwater superoleophobic property under visible optical drive
Can, it is recycled at least through 110 water-oil separating.Show super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film in visible light
There is the regeneration cycle ability of excellent pollution resistance ability, good stability and brilliance under driving.
Illustrate: above embodiments are only to illustrate the present invention and not limit the technical scheme described by the invention；Therefore,
Although this specification is referring to above-mentioned each embodiment, the present invention has been described in detail, the common skill of this field
Art personnel should be appreciated that and still can modify to the present invention or equivalent replacement；And all do not depart from spirit of the invention and
The technical solution and its improvement of range, should all cover in scope of the presently claimed invention.
Claims (7)
1. a kind of preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film, which is characterized in that steps are as follows:
(1) firstly, dispersing n,N-Dimethylformamide in isopropanol, four tincture ester of metatitanic acid is added, after stirring, six hydrations are added
Cobalt chloride, stirring, obtains mixed liquor；
(2) by carbon cloth immersion step (1) obtained mixed liquor, then, by mixed liquor move in ptfe autoclave into
Row heating reaction, cooled to room temperature, obtains super hydrophilic/underwater superoleophobic visible light after reaction after cleaned, dry
Drive pollution resistance film.
2. the preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of one kind according to claim 1,
It is characterized in that, the dosage of n,N-Dimethylformamide described in step (1), isopropanol, metatitanic acid four tincture ester and cobalt chloride hexahydrate
Than for 10~30mL:20~40mL:1~3mL:16~48mg.
3. the preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of one kind according to claim 1,
It is characterized in that, mixing time described in step (1) is 15min.
4. the preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of one kind according to claim 1,
It is characterized in that, temperature described in step (2) is 180~220 DEG C, and the time is 18~22h.
5. the preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of one kind according to claim 1,
It is characterized in that, cleaning described in step (2) is rinsed well with deionized water.
6. the preparation method of super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of one kind according to claim 1,
It is characterized in that, vacuum drying temperature described in step (2) is 60 DEG C, time 6h.
7. by super hydrophilic/underwater superoleophobic visible optical drive pollution resistance film of the described in any item method preparations of claim 1~6
Applied to the water-oil separating in oil-containing water body.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433671A (en) * | 2019-07-23 | 2019-11-12 | 江苏大学 | A kind of preparation method and its usage of visible light-inducing automatically cleaning carbon-fiber film |
| CN112494997A (en) * | 2020-10-23 | 2021-03-16 | 浙江海洋大学 | Porous super-hydrophilic oleophobic material |
| CN115012205A (en) * | 2022-07-01 | 2022-09-06 | 西安理工大学 | Preparation method of renewable carbon fiber super-hydrophilic/super-oleophobic material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103638930A (en) * | 2013-11-28 | 2014-03-19 | 陕西科技大学 | Preparation method and application of CO<2+>-doped titanium dioxide self-cleaning film |
| CN108516607A (en) * | 2018-03-29 | 2018-09-11 | 武汉大学苏州研究院 | A kind of oil hydrosol separation method and the filter membrane for oil hydrosol separation |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638930A (en) * | 2013-11-28 | 2014-03-19 | 陕西科技大学 | Preparation method and application of CO<2+>-doped titanium dioxide self-cleaning film |
| CN108516607A (en) * | 2018-03-29 | 2018-09-11 | 武汉大学苏州研究院 | A kind of oil hydrosol separation method and the filter membrane for oil hydrosol separation |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110433671A (en) * | 2019-07-23 | 2019-11-12 | 江苏大学 | A kind of preparation method and its usage of visible light-inducing automatically cleaning carbon-fiber film |
| CN110433671B (en) * | 2019-07-23 | 2021-09-10 | 江苏大学 | Preparation method and application of visible light induced self-cleaning carbon fiber film |
| CN112494997A (en) * | 2020-10-23 | 2021-03-16 | 浙江海洋大学 | Porous super-hydrophilic oleophobic material |
| CN115012205A (en) * | 2022-07-01 | 2022-09-06 | 西安理工大学 | Preparation method of renewable carbon fiber super-hydrophilic/super-oleophobic material |
| CN115012205B (en) * | 2022-07-01 | 2024-05-03 | 西安理工大学 | Preparation method of renewable carbon fiber super-hydrophilic/super-oleophobic material |
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Application publication date: 20190426 |