CN102029080B - 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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- CN102029080B CN102029080B CN 201010531780 CN201010531780A CN102029080B CN 102029080 B CN102029080 B CN 102029080B CN 201010531780 CN201010531780 CN 201010531780 CN 201010531780 A CN201010531780 A CN 201010531780A CN 102029080 B CN102029080 B CN 102029080B
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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, affect the adverse consequences of aquatile existence, its environmental pollution that causes has become one of significant problem that affects human lives and production.
The complexity that oily waste water is processed 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 the Focal point and difficult point that oily waste water is administered.
The processing method of oily waste water commonly used can be summarized as four large classes at present: Physical, chemical method, physical-chemical process and biochemical process, but its limitation is arranged.Membrane separation process (Physical) for example, utilize the granule medium filter bed hold back and inertial collision, screening, surface adhesion, poly-and etc. mechanism, can remove oil content in the water but exist fenestra easily to stop up, clean difficulty, operating cost is high, is not suitable for the defectives such as extensive processing.Floatingization of floatation (physical-chemical process) efficient is high, easy to control, technical maturity, but operating cost is high, floor space is large, and oil slick is more difficult, also has a large amount of scum silica frost.In a word, be subjected to the restriction of the 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 process.
Summary of the invention
The object 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 process.
Another object of the present invention is to provide a kind of collection oil droplet material preparation method under water.
Collection among the present invention has the high molecular nanofiber of fluorine-containing organic silicon and the staggered tridimensional network of micron particles on the material surface of oil droplet under water, 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 respectively 178 ° and 160 °, 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 formed stable oil film at material surface, 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, prepared at hydroxylated substrate surface under the normal temperature and had the staggered tridimensional network of nanofiber and micron particles, water content in kind by regulating monomer, concentration, the organic solvent etc. is adjusted 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 under water material preparation method of oil droplet is to adopt liquid phase method to be prepared, and the method may further comprise the steps:
May further comprise the steps:
1) surface cleaning being carried out surface hydroxylation without the substrate of greasy dirt processes;
2) in the glassware that can seal, add the organic solvent that contains the vestige water gaging, immersion is through step 1) carry out the substrate that surface hydroxylation was processed, after dripping fluorine-containing organic trichlorosilane monomer to its concentration in organic solvent and being 0.0001vt%～5vt%, confined reaction 10min～120min under the normal temperature, substrate after will processing is afterwards taken out, be mixed solution and the water cleaning treatment of 1: 1 ethanol and water successively with toluene, ethanol, volume ratio, namely obtain the coarse structure surface at 120 ℃ of lower dry 10min 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;
Described step 1) substrate in is clean glass, silicon, quartz;
Described step 1) substrate in also can be used metal material or macromolecular material;
Described step 1) hydroxylating in is processed: the hydroxylating of glass, silicon, quartz surfaces is processed to adopt will pending substrate to put into by the hydrogen peroxide of 30vt% and the 98vt% concentrated sulfuric acid and is soaked 2h with the solution that 3: 7 volume ratio is mixed into, and cleans and dries; The hydroxylating of metal material and macromolecular material is processed the oxygen plasma treatment method that adopted, and processes 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 under water prepared surface of material preparation method of oil droplet 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 respectively 178 ° and 160 °, the contact angle with oil shows as 0 ° under water.
The present invention has following features:
(1) the collection of the present invention material of oil droplet under water, any Chemical Physics variation does not occur in 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 Automatic-falling or just tear-away with a small amount of water cleaning.
(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 the material preparation method of oil droplet function under water and equipment is simple, cost is low, at normal temperatures one-step method rapid large-area ground preparation, 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 afterwards oil droplet for 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 better embodiment of the present invention technical scheme of the present invention is further described.In embodiment under water with the experiment such as the contact angle test of oil in, prepared surface is take water as medium, the oil of employing is any one in carrene, chloroform, carbon tetrachloride, dichloroethanes or the hexadecane etc.
Embodiment 1
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water, put at last temperature and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet under water.
Collect the material surface stereoscan photograph of 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 afterwards oil droplet for 20 times.
Embodiment 2
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of dimethylbenzene, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 3
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of isopropyl alcohol, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 4
1) surface cleaning is soaked 2h without the silicon chip of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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%, under the normal temperature behind the confined reaction 1h with silicon chip extracting, use successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of toluene, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 5
1) surface cleaning is soaked 2h without the silicon chip of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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%, under the normal temperature behind the confined reaction 1h with silicon chip extracting, use successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of n-butanol, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 6
1) surface cleaning is soaked 2h without the quartz plate of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of n-butanol, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 7
1) macromolecular material being carried out surface hydroxylation with plasma processes.
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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of isopropyl alcohol, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 8
1) with surface cleaning without the metal material of greasy dirt with ethanol, acetone ultrasonic cleaning once, water cleans 3 times afterwards, and 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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 9
1) surface cleaning is soaked 2h without the silicon chip of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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%, under the normal temperature behind the confined reaction 1h with silicon chip extracting, use successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of toluene, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 10
1) surface cleaning is soaked 2h without the quartz plate of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of dimethylbenzene, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 11
1) surface cleaning is soaked 2h without the quartz plate of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 12
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 13
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of n-butanol, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 14
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of isopropyl alcohol, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 15
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 16
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively mixed solution (volume ratio is 1: 1) and the water flushing of dimethylbenzene, ethanol, second alcohol and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 17
1) surface cleaning is soaked 2h without the silicon chip of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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%, under the normal temperature behind the confined reaction 1h with silicon chip extracting, use successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Embodiment 18
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water, put at last temperature and be 120 ℃ the dry 10min of drying box, obtain collecting the material of oil droplet 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 afterwards oil droplet for 20 times.
Embodiment 19
1) surface cleaning is soaked 2h without the sheet glass of greasy dirt in the mixed solution (volume ratio is 3: 7) of 30% hydrogen peroxide and the concentrated sulfuric acid, 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 successively respectively the flushing of the mixed solution (volume ratio is 1: 1) of toluene, ethanol, second alcohol and water and water, put at last temperature 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 afterwards oil droplet for 20 times.
Claims (1)
1. collect the material preparation method of oil droplet under water for one kind, may further comprise the steps:
1) surface cleaning being carried out surface hydroxylation without the substrate of greasy dirt processes;
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 processed through step 1), after dripping fluorine-containing organic trichlorosilane monomer to its concentration in organic solvent and being 0.0001vt%～5vt%, confined reaction 10min～120min under the normal temperature, substrate after will processing is afterwards taken out, be mixed solution and the water cleaning treatment of ethanol and the water of 1:1 successively with toluene, ethanol, volume ratio, namely obtain the coarse structure surface at 120 ℃ of lower dry 10min at last;
Described fluorine-containing organic trichlorosilane monomer is trifluoro propyl trichlorosilane, 1H, 1H, 2H, 2H-perfluor decyltrichlorosilane, 1H, 1H, 2H, a kind of in the 2H-perfluoro capryl trichlorosilane or more than a kind of mixture;
Substrate in the described step 1) is clean glass, silicon, quartz, metal material or macromolecular material;
Hydroxylating in the described step 1) is processed: the hydroxylating of glass, silicon, quartz surfaces is processed to adopt will pending substrate to put into by the hydrogen peroxide of 30vt% and the 98vt% concentrated sulfuric acid and is soaked 2h with the solution that the volume ratio of 3:7 is mixed into, and cleans and dries; The hydroxylating of metal material and macromolecular material is processed and has been adopted the oxygen plasma treatment method, processes 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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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010531780 CN102029080B (en) | 2010-10-29 | 2010-10-29 | Underwater oil droplet collection material and method for preparing same |
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| CN 201010531780 CN102029080B (en) | 2010-10-29 | 2010-10-29 | Underwater oil droplet collection material and method for preparing same |
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| CN102029080A CN102029080A (en) | 2011-04-27 |
| CN102029080B true CN102029080B (en) | 2013-02-13 |
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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 |
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