CN107080975A - The preparation method of oil-water separation mesh film with superhydrophilic superoleophobic property - Google Patents
The preparation method of oil-water separation mesh film with superhydrophilic superoleophobic property Download PDFInfo
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- CN107080975A CN107080975A CN201710450108.4A CN201710450108A CN107080975A CN 107080975 A CN107080975 A CN 107080975A CN 201710450108 A CN201710450108 A CN 201710450108A CN 107080975 A CN107080975 A CN 107080975A
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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
- B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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Abstract
The present invention is a kind of preparation method of the oil-water separation mesh film with superhydrophilic superoleophobic property.This method is used as substrate using the wire netting of 400~2000 mesh, using the method for cold spraying, the spray coating hydrophilic material on the twine of wire netting, described hydrophilic material is the one or more in zinc oxide, silica, calcium carbonate and titanium dioxide, and particle size range is 5~200 nanometers；Sintered 60~240 minutes at last 300 DEG C~750 DEG C, obtain the oil-water separation mesh film with superhydrophilic superoleophobic property.The present invention improves adhesion without being modified modification in itself to wire netting without adhesive, will not produce secondary pollution, and cleaning is easy, may be reused.
Description
Technical field
The invention belongs to chemical, technical field of function materials, and in particular to the oil with superhydrophilic superoleophobic property
The preparation method and purposes of moisture off-network film.
Background technology
In the last few years, developing rapidly with industry, oilfield exploitation scale constantly expands, the oily waste water that plant produced is produced
Water is also being continuously increased, the problem of water-oil separating is had become with people's lives, economic development and closely bound up environmental protection.One
Aspect, the field such as food processing, metal smelt, petrochemical industry, weaving generates substantial amounts of industrial oily waste water, and these are to environment
Very serious pollution will be caused；On the other hand, with the exploitation of submarine oil, oil leakage phenomenon is also serious all the more, and this is to sea
Foreign environment will also result in larger pollution.So how to realize that profit is efficiently separated turns into that today's society is urgently to be resolved hurrily asks
Topic, the oil-water separating net with special wellability gradually receives the concern of people.
Document Angew.Chem.Int.Ed., 2004,43,2012-2014；J.Chem.Technol.Biotechnol,
2012,87,427-430；Appl.Surf.Sci.,2007,253(23),9054-9060；Appl.Surf.Sci.,2008.254
(18), 6002-6006 reports the nethike embrane with super-hydrophobic super-oleophylic property for water-oil separating.Although net reported above
Film all has the effect of water-oil separating, but there is also different deficiencies, such as manufacturing process is complex, and what is had also needs high temperature to consolidate
Change, what is had has used fluorochemical, separation of oil water mixture not being suitable for containing a small amount of oil in a large amount of water having etc..
In current techniques such as CN104759118A, CN104689602A, make adhesive partially cured on wire netting first,
Then the micro-nano prepared by series reaction is combined into polyhedron suspension using cold spray-coating method to be coated on wire netting, treated
Dispersion liquid volatilization is complete, that is, obtains oil-water separation mesh film.The oil-water separation mesh film that this method is obtained is super-hydrophobic super-oleophylic, so
And because lipophile nethike embrane is particularly easy to contaminated or even blocked, especially highly viscous oil can have a strong impact on separative efficiency, and
And the oil of adhesion is difficult to clean off, cause the secondary pollution in aftertreatment technology, nethike embrane is difficult to reuse.While the system of this method
Make process complex, be difficult large area low cost production.
The content of the invention
The purpose of the present invention is that have for deficiency present in current techniques there is provided a kind of inexpensive, simple and convenient
The preparation method of the oil-water separation mesh film of superhydrophilic superoleophobic property.The profit with superhydrophilic superoleophobic property point of the present invention
Off-network film is, using the wire netting of 400~2000 mesh as substrate, using the method for cold spraying, parent to be coated on the twine of wire netting
Water-based material, adhesion is improved by high temperature sintering, without being modified modification in itself to wire netting, is improved and is tied without adhesive
With joint efforts, so as to obtain the oil-water separation mesh film with superhydrophilic superoleophobic property.The present invention will not produce secondary pollution, and cleaning is held
Easily, it may be reused.
The technical scheme is that：
A kind of preparation method of the oil-water separation mesh film with superhydrophilic superoleophobic property, comprises the following steps：
(1) wire netting of 400~2000 mesh is cleaned by ultrasonic, then dried at room temperature；
(2) by water wetted material in tetrahydrofuran ultrasonic disperse 60~180 minutes, the aaerosol solution stablized；
Wherein, the weight/mass percentage composition of water wetted material is 0.5~3.8% in aaerosol solution；Described hydrophilic material is
One or more in zinc oxide, silica, calcium carbonate and titanium dioxide, particle size range is 5~200 nanometers；
(3) aaerosol solution is obtained into dried metal using the gases at high pressure even application of air compressor machine into step (1)
The surface of net；The nozzle bore of spray gun is 1.0mm, and the air compressor pressure of connection spray gun is 0.3-0.6MPa, the spray of spray gun
It is 10~20cm to apply distance；Spraying 0.5~6.8g aaerosol solutions every square centimeter；
(4) wire netting of step (3) spray coated suspension is aged 30~90 minutes at room temperature, last 300 DEG C~750
Sintered 60~240 minutes at DEG C, obtain the oil-water separation mesh film with superhydrophilic superoleophobic property.
Cleaning in described step (1) is specially cleaned by ultrasonic with acetone, isopropanol and deionized water successively.
Described wire netting is stainless (steel) wire, copper mesh or iron net.
Beneficial effects of the present invention are：
The oil-water separation mesh film of the present invention has special micro-nano compound structure：The mesh and twine of micro-meter scale, nanometer
The water wetted material of yardstick.The oil-water separation mesh film of the present invention is hydrophilic in atmosphere, first with water complete wetting nethike embrane, works as net
Film is by after water complete wetting, and water is filled into the micro-nano compound structure on twine surface, when oil water mixture touches water-oil separating
During nethike embrane, water smoothly can be permeated by hole, and oil is repelled by the moisture film on oil-water separation mesh film surface, is trapped in oil-water separation mesh film
Top, realizes water-oil separating purpose.The oil-water separation mesh film of the present invention is in atmosphere to the contact angle of water droplet close to 0 °, under water
150 ° are more than to the contact angle of oil droplet.
The raw material of the oil-water separation mesh film of the present invention are cheap and easy to get, and equipment and manufacturing process are simple, can be low with large area
Cost is produced.The water flux of the oil-water separation mesh film of the present invention is big, and water-oil separating speed is fast, to the separative efficiency of oil water mixture
Up to 99.9%, it is adaptable to the big wastewater treatment of oil content, to n-hexane, kerosene, petroleum ether, benzene, dichloroethanes, diesel oil, dynamic
Vegetable oil, gasoline and crude oil etc. have good separating effect.Available for the water-oil separating of oily waste water, such as it can be used for containing food
With the water-oil separating of the oily waste waters such as oil, oil, kerosene.
The oil-water separation mesh film meets current social development demand without poisonous and harmful substance, easily cleaning, repeatable to make
With.
Brief description of the drawings
The stereoscan photograph of oil-water separation mesh film prepared by Fig. 1 embodiment of the present invention 1；
The contact angle of oil-water separation mesh film prepared by Fig. 2 embodiment of the present invention 1 in atmosphere to water droplet；
The contact angle of oil-water separation mesh film prepared by Fig. 3 embodiment of the present invention 1 under water to oil droplet；
Oil-water separation mesh film prepared by Fig. 4 embodiment of the present invention 1 is used for the experimental provision of water-oil separating and experiment effect shines
Piece；Wherein,
1. the oil after separation；2. by the oil-water separation mesh film of water complete wetting；3. the water after separation.
Embodiment
Embodiment 1.
(1) stainless (steel) wire (5 5 centimetres of cm x) of 1000 mesh (aperture is 15 μm) is immersed into acetone successively, isopropanol and
It is each in deionized water to be cleaned by ultrasonic 10 minutes, dry at room temperature；
(2) at room temperature, 1g titanium dioxide (8 nanometers of particle diameter), 150ml tetrahydrofurans are added in 250ml single port bottles
(133.4g), ultrasound obtains the stable aaerosol solutions of 134.4g for 60 minutes；
(3) aaerosol solution for obtaining step (2) is dried not to (1) using the gases at high pressure even application of air compressor machine
The surface of rust steel mesh；The nozzle bore of spray gun is 1.0mm, and the air compressor pressure of connection spray gun is maintained at 0.4MPa, sprayed
Distance is 16cm.
(4) stainless (steel) wire of step (3) spray coated suspension is aged 30 minutes at room temperature, finally burnt at 550 DEG C
Knot 150 minutes, obtains the oil-water separation mesh film with superhydrophilic superoleophobic property, and there is gained oil-water separation mesh film aperture to be about
15 microns of mesh (as shown in Figure 1)；
(5) the oil-water separation mesh film surface that measuring process (4) is obtained in atmosphere is approached to the contact angle of 10 microlitres of water droplets
0 ° (as shown in Figure 2)；The oil-water separation mesh film surface is measured under water, and 150 ° of (such as Fig. 3 are more than to the contact angle of 10 microlitres of kerosene
It is shown)；
(6) water-oil separating experiment is carried out using the experimental provision shown in Fig. 4.Water complete wetting oil obtained above is used first
(described complete wetting is that each several part of oil-water separation mesh film 2 touches water to moisture off-network film 2, such as by oil-water separating net
Film 2 takes out at once after being submerged into water.Following examples are same), then nethike embrane 2 is clipped in the middle of glass tube, by kerosene and water
Mixture (volume ratio 1:1, magnetic agitation 20 minutes) it is poured in above-mentioned oil-water separation mesh film, after nethike embrane is by water complete wetting,
Water is filled into the micro-nano compound structure on twine surface, and when oil water mixture touches oil-water separation mesh film, water can be quick
Through oil-water separation mesh film, the water 3 after being separated；Kerosene is repelled by the moisture film on oil-water separation mesh film surface simultaneously, is trapped in
Above oil-water separation mesh film, the oil 1 after being separated realizes water-oil separating purpose, and water-oil separating rate is 99.9%.
The present invention separating mechanism be：
The oil-water separation mesh film of the present invention not only has hydrophily, and with special micro-nano compound structure, this causes
Adhesion strength is more than the cohesive strength of water in itself when water is contacted with nanometer protrusion surface, so as to enable water in oil-water separation mesh film
Capillary canal in produce stick pull effect and form liquid bridge, while the effect of mass transmitting based on liquid bridge makes water continually pass
Pass.And the liquid film formed by water serves the effect of isolation mass transfer to oil, so that oil can not touch oil-water separating net
The surface of film, realizes water-oil separating purpose.
Embodiment 2.
(1) copper mesh (5 5 centimetres of cm x) of 800 mesh (aperture is 19 microns) is immersed into acetone successively, isopropanol and go from
It is each in sub- water to be cleaned by ultrasonic 10 minutes, dry at room temperature；
(2) at room temperature, 1g zinc oxide (10 nanometers of particle diameter), 0.5g silica (particle diameter 15 are added in 250ml single port bottles
Nanometer), 100ml tetrahydrofurans (88.9g), ultrasound obtains the stable aaerosol solutions of 90.4g for 80 minutes；
(3) aaerosol solution for obtaining step (2) using the gases at high pressure even application of air compressor machine to (1) dried copper
The surface of net；The nozzle bore of spray gun is 1.0mm, and the air compressor pressure of connection spray gun is maintained at 0.4MPa, spray distance
For 16cm.
(4) copper mesh of step (3) spray coated suspension is aged 50 minutes at room temperature, 180 points is sintered at last 450 DEG C
Clock, obtains the oil-water separation mesh film with superhydrophilic superoleophobic property, and there is gained oil-water separation mesh film aperture to be about 19 microns
Mesh；
(5) the oil-water separation mesh film surface that measuring process (4) is obtained in atmosphere is approached to the contact angle of 10 microlitres of water droplets
0°；The oil-water separation mesh film surface is measured under water, and 150 ° are more than to the contact angle of 10 microlitres of n-hexanes；
(6) water-oil separating experiment is carried out using the experimental provision shown in Fig. 4.Water complete wetting oil obtained above is used first
Nethike embrane, is then clipped in the middle of glass tube by moisture off-network film, by the mixture (volume ratio 2 of n-hexane and water:3, magnetic agitation 30
Minute) be poured in above-mentioned oil-water separation mesh film, after nethike embrane is by water complete wetting, water is filled into the micro-nano composite junction on twine surface
In structure, when oil water mixture touches oil-water separation mesh film, water can pass rapidly through oil-water separation mesh film, after being separated
Water；N-hexane is repelled by the moisture film on oil-water separation mesh film surface simultaneously, is trapped in above oil-water separation mesh film, after being separated
Oil, realizes water-oil separating purpose.
Embodiment 3.
(1) iron net (5 5 centimetres of cm x) of 400 mesh (aperture is 37 microns) is immersed into acetone successively, isopropanol and go from
It is each in sub- water to be cleaned by ultrasonic 10 minutes, dry at room temperature；
(2) at room temperature, 1g zinc oxide (20 nanometers of particle diameter) is added in 250ml single port bottles, 0.5g calcium carbonate (receive by particle diameter 16
Rice), 0.5g silica (21 nanometers of particle diameter), 150ml tetrahydrofurans (133.4g), it is stable that ultrasound obtains 135.4g for 120 minutes
Aaerosol solution；
(3) aaerosol solution for obtaining step (2) using the gases at high pressure even application of air compressor machine to (1) dried iron
The surface of net；The nozzle bore of spray gun is 1.0mm, and the air compressor pressure of connection spray gun is maintained at 0.4MPa, spray distance
For 16cm.
(4) iron net of step (3) spray coated suspension is aged 70 minutes at room temperature, 240 points is sintered at last 350 DEG C
Clock, obtains the oil-water separation mesh film with superhydrophilic superoleophobic property, and there is gained oil-water separation mesh film aperture to be about 37 microns
Mesh；
(5) the oil-water separation mesh film surface that measuring process (4) is obtained in atmosphere is approached to the contact angle of 10 microlitres of water droplets
0°；The oil-water separation mesh film surface is measured under water, and 150 ° are more than to the contact angle of 10 microlitres of edible oils；
(6) water-oil separating experiment is carried out using the experimental provision shown in Fig. 4.Water complete wetting oil obtained above is used first
Nethike embrane, is then clipped in the middle of glass tube by moisture off-network film, by the mixture (volume ratio 2 of edible oil and water:3, magnetic agitation 30
Minute) be poured in above-mentioned oil-water separation mesh film, after nethike embrane is by water complete wetting, water is filled into the micro-nano composite junction on twine surface
In structure, when oil water mixture touches oil-water separation mesh film, water can pass rapidly through oil-water separation mesh film, after being separated
Water；Edible oil is repelled by the moisture film on oil-water separation mesh film surface simultaneously, is trapped in above oil-water separation mesh film, after being separated
Oil, realizes water-oil separating purpose.
Embodiment 4
It will carry out drying at room temperature after the oil-water separation mesh film after water-oil separating is cleaned with ethanol in embodiment 1, enter again
Row water-oil separating.Separating effect still can reach 99.9% after recycling 20 times.
Above test result indicates that, oil-water separation mesh film of the invention in atmosphere to the contact angle of water droplet close to 0 ° (such as
Shown in Fig. 2), water smoothly can be permeated by hole；Oil-water separation mesh film is under water to oil droplet (such as n-hexane, kerosene, oil simultaneously
Ether, benzene, dichloroethanes, diesel oil, vegetable and animals oils, gasoline and crude oil etc.) contact angle be more than 150 ° (as shown in Figure 3), oil
The oil-water separation mesh film surface of invention can not infiltrate, and be trapped in above nethike embrane.Hydrophilic material water absorbing properties are good, and water can be smooth
By oil-water separation mesh film, and oil is completely blocked above oil-water separation mesh film, so as to realize stabilization, efficient profit point
From effect.Because the oil-water separation mesh film of the present invention is more than 150 ° to the contact angle of oil droplet under water, mesh is difficult to be blocked up by oil droplet
Plug, the described oil-water separation mesh film after use is easy to clean, may be reused.
Unaccomplished matter of the present invention is known technology.
Claims (3)
1. a kind of preparation method of the oil-water separation mesh film with superhydrophilic superoleophobic property, it is characterized in that this method is including following
Step：
（1）The wire netting of 400 ~ 2000 mesh is cleaned by ultrasonic, then dried at room temperature；
（2）By water wetted material in tetrahydrofuran ultrasonic disperse 60 ~ 180 minutes, the aaerosol solution stablized；
Wherein, the weight/mass percentage composition of water wetted material is 0.5 ~ 3.8% in aaerosol solution；Described hydrophilic material be zinc oxide,
One or more in silica, calcium carbonate and titanium dioxide, particle size range is 5 ~ 200 nanometers；
（3）By aaerosol solution using the gases at high pressure even application of air compressor machine to step（1）In obtain dried wire netting
Surface；The air compressor pressure for connecting spray gun is 0.3 ~ 0.6MPa, and the spray distance of spray gun is 10 ~ 20cm；It is every square centimeter
Spray 0.5 ~ 6.8g aaerosol solutions；
（4）By step（3）The wire netting of spray coated suspension is aged 30 ~ 90 minutes at room temperature, is burnt at last 300 DEG C ~ 750 DEG C
Knot 60 ~ 240 minutes, obtains the oil-water separation mesh film with superhydrophilic superoleophobic property.
2. there is the preparation method of the oil-water separation mesh film of superhydrophilic superoleophobic property as claimed in claim 1, it is characterized in that
Described step（1）In cleaning be specially cleaned by ultrasonic respectively with acetone, isopropanol and deionized water.
3. there is the preparation method of the oil-water separation mesh film of superhydrophilic superoleophobic property as claimed in claim 1, it is characterized in that
Described wire netting is stainless (steel) wire, copper mesh or iron net.
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