CN102029080A - Underwater oil droplet collection material and method for preparing same - Google Patents
Underwater oil droplet collection material and method for preparing same Download PDFInfo
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Abstract
The invention belongs to the field of the oil absorption material and particularly relates to an underwater oil droplet collection material and a method for preparing the same. Fluorine-containing organic trichlorosilane monomers and a small quantity of water are used as raw materials, and the fluorine-containing organic trichlorosilane monomers are grafted and subjected to hydrolysis and condensation reaction on the surface of a substrate so that the surface in the micron-particle and nano-fiber interlaced three-dimensional network structure is prepared at normal temperature in one step. Underwater oil droplets spread on the surface of the underwater oil droplet collection material so that a stable oil film is formed on the surface of the underwater oil droplet collection material and oil droplets are collected. The method for preparing the underwater oil droplet collection material adopts simple equipment, has low cost, can not cause pollution to environment and can be used for rapidly preparing the underwater oil droplet collection material in a larger area at normal temperature in one step. The prepared functional film has good oil droplet collection function, and the underwater oil droplet collection material can be used repeatedly.
Description
Technical field
The invention belongs to the oil absorption material field, particularly collect material of oil droplet under water and preparation method thereof.
Background technology
Oily waste water is a kind ofly to have a large capacity and a wide range and endanger serious pollution sources, is mainly derived from petrochemical industry, mechanical industry and marine transportation industry.If oily waste water is not recycled, can cause and enter river, lake or bay polluted-water, influence the adverse consequences of aquatile existence, its environmental pollution that causes has become one of significant problem that influences human lives and production.
The complexity that oily waste water is handled depends on source, composition and the existence form of oil content.Oil content in the oily waste water exists with oil slick, dispersed oil, oil emulsion and dissolving wet goods form usually.The oil droplet size of oil slick greater than 100 μ m, is easy to separate from waste water usually; Dispersed oil easily is converted into oil slick or oil emulsion; The oil emulsion oil droplet size is emulsified state less than 10 μ m, stable for extended periods of time state and be difficult for separating from waste water.Therefore the removal of oil emulsion is emphasis and the difficult point that oily waste water is administered.
The processing method of oily waste water commonly used can reduce four big classes at present: physics method, chemical method, physical-chemical process and biochemical process, but its limitation is all arranged.Membrane separation process (physics method) for example utilizes holding back and mechanism such as inertial collision, screening, surface adhesion, coalescence of granule medium filter bed, can remove oil content in the water but exists fenestra easily to stop up, and cleans difficulty, operating cost is high, is not suitable for defectives such as extensive processing.Floatingization of floatation (physical-chemical process) efficient height, easy to control, technical maturity, but operating cost height, floor space are big, and oil slick is more difficult, also has a large amount of scum silica frost.In a word, be subjected to the restriction of conditions such as subsequent treatment, recycling and financial cost, these methods all are difficult to the effect that reaches satisfied, and it is imperative to improve the new technology that conventional method or exploitation oily waste water handle.
Summary of the invention
The objective of the invention is to develop a kind of collection material of oil droplet under water, the new approaches that provide a kind of oily waste water to handle.
Another object of the present invention is to provide a kind of collection oil droplet preparation methods under water.
Collection among the present invention has the nanofiber and the staggered tridimensional network of micron particles of fluorine-containing organosilicon macromolecule under water on the material surface of oil droplet, its nanofiber is of a size of diameter 50～200nm, the diameter of micron particles is 0.5～5 μ m, its coarse structure surface shows as super two characteristic of dredging in air, contact angle with water and oil in air reaches 178 ° and 160 ° respectively, under water since three-dimensional netted coarse groove colligation air, formed the interface of air-water, oil droplet is sprawled after the air-water interface contact, contact angle shows as 0 °, thereby on material surface, formed stable oil film, further reached the effect of collecting oil droplet.
For solving above-mentioned purpose, the present invention has adopted following technical scheme:
Utilize the hydrolysis condensation reaction of fluorine-containing organic trichlorosilane monomer, on hydroxylated substrate surface, prepared under the normal temperature and had nanofiber and the staggered tridimensional network of micron particles, water content in kind by regulating monomer, concentration, the organic solvent waits adjusts surface texture, thereby makes the surface of solids reach the function of aerial ultra-amphosphobic and underwater collection oil droplet.
The collection of the present invention material preparation method of oil droplet under water is to adopt liquid phase method to be prepared, and this method may further comprise the steps:
May further comprise the steps:
1) the surface hydroxylation processing is carried out in the substrate of surface cleaning not being had greasy dirt;
2) in the glassware that can seal, add the organic solvent that contains the vestige water gaging, immersion is carried out the substrate that surface hydroxylation was handled through step 1), drip after fluorine-containing organic trichlorosilane monomer to its concentration in organic solvent is 0.0001vt%～5vt%, confined reaction 10min～120min under the normal temperature, substrate after will handling is afterwards taken out, be the mixed solution and the water cleaning treatment of 1: 1 ethanol and water successively with toluene, ethanol, volume ratio, dry 10min promptly obtains the coarse structure surface under 120 ℃ at last;
Described fluorine-containing organic trichlorosilane monomer is trifluoro propyl trichlorosilane, 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane and in a kind of or more than a kind of mixture;
Substrate in the described step 1) is clean glass, silicon, quartz;
Substrate in the described step 1) also can be used metal material or macromolecular material;
Hydroxylating in the described step 1) is handled: the hydroxylating of glass, silicon, quartz surfaces is handled and is adopted the hydrogen peroxide and the 98vt% concentrated sulfuric acid that pending substrate is put into by 30vt% to soak 2h with the composite solution of 3: 7 volume ratio, cleans oven dry; The hydroxylating of metal material and macromolecular material is handled the oxygen plasma treatment method that adopted, and handles 5～20min under the pressure conditions of～50mtorr;
Described step 2) organic solvent in is toluene, dimethylbenzene, isopropyl alcohol or n-butanol;
The water of the trace described step 2) is that the content of water in organic solvent is 0～10ppm;
The above-described collection prepared surface of material preparation method of oil droplet under water has nanofiber and the staggered three-dimensional netted coarse structure of micron particles, it is 50～200nm that its nanofiber is of a size of diameter, the diameter of micron particles is 0.5～5 μ m, its coarse structure surface in air with water and oil contact angle reach 178 ° and 160 ° respectively, the contact angle with oil shows as 0 ° under water.
The present invention has following characteristics:
(1) the collection of the present invention material of oil droplet under water, any Chemical Physics variation does not take place in back material itself before use, when collecting oil under water, because its special surface texture, oil is sprawled into stable oil film at material surface, after taking out from water, the oil film of sprawling can come off automatically or clean just tear-away with low amounts of water.
(2) this surface has novel special surface wettability.
(3) collection of the present invention is expected to fields such as administering the water pollution in the surface of oil droplet function under water.
(4) the present invention collects under water oil droplet materials with function preparation method and equipment is simple, cost is low, one-step method rapid large-area ground preparation at normal temperatures, compares with traditional oily waste water material for water treatment and can not bring secondary pollution, can repeatedly recycle.
Utilize the collection oil droplet function of the prepared functional membrane of the method for the invention good, material can repeatedly recycle.Prepared functional membrane can be collected oil 0.1～10ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Description of drawings
The present invention has accompanying drawing 2 width of cloth:
Fig. 1 collects the material surface stereoscan photograph of oil droplet under water;
Fig. 2 collects under water that the material of oil droplet contacts forward and backward contact angle figure under water with oil droplet.
The specific embodiment
Below in conjunction with preferable embodiment of the present invention technical scheme of the present invention is further described.In embodiment under water with experiment such as the contact angle test of oil in, prepared surface is medium with water, the oil of employing is any one in carrene, chloroform, carbon tetrachloride, dichloroethanes or the hexadecane etc.
Embodiment 1
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the toluene of 1ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane is mixed with the solution that concentration is 0.5vt%, behind the confined reaction 1h sheet glass is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The material surface stereoscan photograph of collecting oil droplet under water as shown in Figure 1; The marine material surface contacts forward and backward contact angle figure as shown in Figure 2 with oil droplet.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 6～8ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 2
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the dimethylbenzene of 5ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane is mixed with the solution that concentration is 5vt%, behind the confined reaction 1h sheet glass is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of dimethylbenzene, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 9～10ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 3
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the isopropyl alcohol of 0ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane is mixed with the solution that concentration is 0.0001vt%, behind the confined reaction 1h sheet glass is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of isopropyl alcohol, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 0.1～1ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 4
1) silicon chip that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the silicon chip sheet of handling well is immersed into 10mL is in the toluene of 10ppm, wherein drip the trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 5vt%, behind the confined reaction 1h silicon chip is taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of toluene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 6～8ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 5
1) silicon chip that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the silicon chip of handling well is immersed into 10mL is in the n-butanol of 8ppm, wherein drip 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane is mixed with the solution that concentration is 4vt%, behind the confined reaction 1h silicon chip is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of n-butanol, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 3～6ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 6
1) quartz plate that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the quartz plate of handling well is immersed into 10mL is in the n-butanol of 2ppm, wherein drip 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane is mixed with the solution that concentration is 0.1vt%, behind the confined reaction 1h quartz plate is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of n-butanol, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 1～2ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 7
1) macromolecular material being carried out surface hydroxylation with plasma handles.
2) water content that the macromolecular material of handling well is immersed into 10mL is in the isopropyl alcohol of 3ppm, wherein drip 1H, 1H, 2H, the mixture of 2H-perfluor decyltrichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 3vt%, behind the confined reaction 1h macromolecular material is taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of isopropyl alcohol, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 3～5ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 8
1) metal material that surface cleaning is not had a greasy dirt with ethanol, acetone ultrasonic cleaning once, water cleans 3 times afterwards, nitrogen dries up.
2) water content that the metal material of handling well is immersed into 10mL is in the dimethylbenzene of 9ppm, wherein drip 1H, 1H, 2H, the mixture of 2H-perfluoro capryl trichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 5vt%, behind the confined reaction 1h metal material is taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 4～6ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 9
1) silicon chip that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the silicon chip of handling well is immersed into 10mL is in the toluene of 4ppm, wherein drip the trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 1vt%, behind the confined reaction 1h silicon chip is taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of toluene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 4～5ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 10
1) quartz plate that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the dimethylbenzene of 6ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane is mixed with the solution that concentration is 1vt%, behind the confined reaction 1h quartz plate is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of dimethylbenzene, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 4～5ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 11
1) quartz plate that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the quartz plate of handling well is immersed into 10mL is in the toluene of 6ppm, wherein drip 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane is mixed with the solution that concentration is 1vt%, behind the confined reaction 1h quartz plate is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 5～6ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 12
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the dimethylbenzene of 1ppm, wherein drip 1H, 1H, 2H, the mixture of 2H-perfluor decyltrichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 0.5vt%, behind the confined reaction 1h sheet glass is taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 1～2ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 13
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the n-butanol of 10ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, the mixture of 2H-perfluoro capryl trichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 5vt%, behind the confined reaction 1h sheet glass taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of n-butanol, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 8～10ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 14
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the isopropyl alcohol of 5ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, the mixture of 2H-perfluoro capryl trichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 2.5vt%, behind the confined reaction 1h sheet glass taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of isopropyl alcohol, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 5～8ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 15
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the dimethylbenzene of 2ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, the mixture of 2H-perfluoro capryl trichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 1.5vt%, behind the confined reaction 1h sheet glass taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 1～3ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 16
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the dimethylbenzene of 5ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, the mixture of 2H-perfluoro capryl trichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 5vt%, behind the confined reaction 1h sheet glass taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 5～8ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 17
1) silicon chip that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the silicon chip of handling well is immersed into 10mL is in the toluene of 2ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, the mixture of 2H-perfluoro capryl trichlorosilane and trifluoro propyl trichlorosilane, be mixed with the solution that concentration is 2vt%, behind the confined reaction 1h silicon chip taken out under the normal temperature, use the mixed solution (volume ratio is 1: 1) and the water flushing of toluene, ethanol, second alcohol and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 4～6ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 18
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the toluene of 2ppm, wherein drip 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane is mixed with the solution that concentration is 0.2vt%, behind the confined reaction 1h sheet glass is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting oil droplet materials with function under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 2～3ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Embodiment 19
1) sheet glass that surface cleaning is not had a greasy dirt soaks 2h in the mixed solution (volume ratio is 3: 7) of 30% the hydrogen peroxide and the concentrated sulfuric acid, and water cleans 3 times afterwards, and nitrogen dries up.
2) water content that the sheet glass of handling well is immersed into 10mL is in the dimethylbenzene of 2ppm, wherein drip 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane is mixed with the solution that concentration is 0.1vt%, behind the confined reaction 1h sheet glass is taken out under the normal temperature, use the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water respectively successively, put into temperature at last and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
The marine material surface is 0 ° with the contact angle of oil droplet.This material can be collected oil 1～2ml/cm at every turn under water
2, it is still good to recycle the function of collecting oil droplet after 20 times.
Claims (2)
1. collect the material of oil droplet under water for one kind, it is characterized in that: described collection has the nanofiber and the staggered tridimensional network of micron particles of fluorine-containing organosilicon macromolecule under water on the material surface of oil droplet, its nanofiber is of a size of diameter 50～200nm, the diameter of micron particles is 0.5～5 μ m, its coarse structure surface shows as super two characteristic of dredging in air, contact angle with water and oil in air reaches 178 ° and 160 ° respectively, under water since three-dimensional netted coarse groove colligation air, formed the interface of air-water, oil droplet is sprawled after the air-water interface contact, contact angle shows as 0 °, thereby on material surface, formed stable oil film, further reached the effect of collecting oil droplet.
2. collect the material preparation method of oil droplet under water for one kind, may further comprise the steps:
1) the surface hydroxylation processing is carried out in the substrate of surface cleaning not being had greasy dirt;
2) in the glassware that can seal, add the organic solvent that contains the vestige water gaging, immersion is carried out the substrate that surface hydroxylation was handled through step 1), drip after fluorine-containing organic trichlorosilane monomer to its concentration in organic solvent is 0.0001vt%～5vt%, confined reaction 10min～120min under the normal temperature, substrate after will handling is afterwards taken out, be the mixed solution and the water cleaning treatment of 1: 1 ethanol and water successively with toluene, ethanol, volume ratio, dry 10min promptly obtains the coarse structure surface under 120 ℃ at last;
Described fluorine-containing organic trichlorosilane monomer is trifluoro propyl trichlorosilane, 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane and in a kind of or more than a kind of mixture;
Substrate in the described step 1) is clean glass, silicon, quartz;
Substrate in the described step 1) also can be used metal material or macromolecular material;
Hydroxylating in the described step 1) is handled: the hydroxylating of glass, silicon, quartz surfaces is handled and is adopted the hydrogen peroxide and the 98vt% concentrated sulfuric acid that pending substrate is put into by 30vt% to soak 2h with the composite solution of 3: 7 volume ratio, cleans oven dry; The hydroxylating of metal material and macromolecular material is handled the oxygen plasma treatment method that adopted, and handles 5～20min under the pressure conditions of～50mtorr;
Described step 2) organic solvent in is toluene, dimethylbenzene, isopropyl alcohol or n-butanol;
The water of the trace described step 2) is that the content of water in organic solvent is 0～10ppm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107362586A (en) * | 2017-07-12 | 2017-11-21 | 平顶山学院 | The preparation method and application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane |
| CN108525970A (en) * | 2018-03-13 | 2018-09-14 | 上海交通大学 | The preparation method of noble metal super-double-hydrophobic surface |
| CN108543686A (en) * | 2018-03-13 | 2018-09-18 | 上海交通大学 | The preparation method of iron group metal super-double-hydrophobic surface |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1721030A (en) * | 2005-06-09 | 2006-01-18 | 南京大学 | Super-hydrophobic/super-oleophilic oil-water separating net |
| CN1931448A (en) * | 2006-09-27 | 2007-03-21 | 中国科学院上海硅酸盐研究所 | Method of forming hydrophobic transparent film on the surface of different substrates |
| CN101708384A (en) * | 2009-11-23 | 2010-05-19 | 吉林大学 | Method for preparing metal mesh for oil-water separation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1721030A (en) * | 2005-06-09 | 2006-01-18 | 南京大学 | Super-hydrophobic/super-oleophilic oil-water separating net |
| CN1931448A (en) * | 2006-09-27 | 2007-03-21 | 中国科学院上海硅酸盐研究所 | Method of forming hydrophobic transparent film on the surface of different substrates |
| CN101708384A (en) * | 2009-11-23 | 2010-05-19 | 吉林大学 | Method for preparing metal mesh for oil-water separation |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107362586A (en) * | 2017-07-12 | 2017-11-21 | 平顶山学院 | The preparation method and application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane |
| CN107362586B (en) * | 2017-07-12 | 2018-09-07 | 平顶山学院 | The preparation method and application of super-hydrophobic super-oleophylic water-oil separating cork filter membrane |
| CN108525970A (en) * | 2018-03-13 | 2018-09-14 | 上海交通大学 | The preparation method of noble metal super-double-hydrophobic surface |
| CN108543686A (en) * | 2018-03-13 | 2018-09-18 | 上海交通大学 | The preparation method of iron group metal super-double-hydrophobic surface |
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