CN106215462A - Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings and preparation method and application - Google Patents
Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings and preparation method and application Download PDFInfo
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- B01D17/02—Separation of non-miscible liquids
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Abstract
Open super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings of the present invention and preparation method and application.First stainless (steel) wire is carried out pretreatment by this preparation method；Then preparation POSS base hydridization acrylate polymer solution, add in the substrate spraying to clean after room temperature fast-curing agent mixes immediately subsequently in prepared polymer solution, obtaining super-hydrophobic/super-oleophilic rustless steel nethike embrane, wherein POSS based polyalcohol is that the method by free radical solution polymerization prepares.The present invention need not use expensive fluorine-containing material, and raw material is easy to get, and synthesis and spraying coating process are simple, can room temperature fast-curing, it is easy to large-scale production.The stainless (steel) wire that the present invention prepares has preferable hydrophobic oleophilic oil characteristic, it is possible to the separation to multiple oily waste water of the realization rapidly and efficiently, this oil-water separation mesh film has preferable stability simultaneously, can realize being recycled for multiple times.
Description
Technical field
The present invention relates to a kind of oil-water separation material, particularly relate to a kind of based on POSS base hydridization acrylate coatings
Super-hydrophobic/super-oleophilic stainless (steel) wire and preparation method thereof and the application in oil-water separation, belong to organic/inorganic hybridization material and
Super hydrophobic material field.
Background technology
The separation method of traditional oily waste water mainly has centrifugal separation, flotation partition method, gravitational separation process, absorption to divide
From method and vacuum separation method, but to there is separation efficiency low for these methods, needs special equipment and the shortcoming such as energy consumption is high.Separately
On the one hand, oily waste water discharge not only serious threat human health in a large number, bring huge the most also can to whole ecological environment
Big harm.Therefore, the separation method of the oily waste water developing a kind of simple highly effective seems particularly important.
In recent years, there is the surface of super-hydrophobic/super-oleophilic characteristic cause and study interest widely, owing to this surface is to oil
Having contrary wettability with water, therefore this surface is capable of the sharp separation of oily waste water.Chinese patent
CN105056577A discloses a kind of three layers of spraying process of employing and PTFE PPS covers prepared super oleophylic on stainless steel cloth
Super-hydrophobic oil-water separation mesh film, and it is used successfully to oil-water separation.Chinese patent CN104725599A discloses a kind of by fluorine-containing list
Body introduces epoxy resin, then by phase reversal, fluorine-containing epoxy resin is made emulsion, this emulsion is solidified on filter paper prepared super
The oil-water separation film of hydrophobic/super oleophylic.But said method all employs fluorine-containing low table energy material, production cost certainly will be caused
Raising and the pollution of environment, therefore need badly and develop the cheap oil-water separation material of a kind of free-floride.
Chinese patent CN103173998A discloses a kind of by modifying excessive metal nanoparticle, then warp at fabric face
Certain density thiol solution prepares superhydrophobic woven fabric after modifying, and can be successfully applied to oil-water separation.Chinese patent
CN105148562A discloses a kind of method first passing through negative electrode electro-deposition and deposits Nanometer Copper on copper mesh surface, more after deposit
Copper mesh surface carries out wax candle ash deposition and obtains the oil-water separation mesh film of superhydrophobic property.Chinese patent CN104525951A discloses
A kind of by the copper fiber felt matrix surface using high temperature solid-phase sintering to prepare, first carry out chemistry under strongly alkaline conditions heavy
Long-pending, then the copper fiber preparing the hydrophobic oleophilic oil with higher oil-water separation efficiency it is chemically modified with stearic acid ethanol solution
Felt.Although above-mentioned oil-water separation mesh film is unused fluorine-containing material in preparation process, but it is loaded down with trivial details to there is preparation process, needs
Wanting the shortcoming such as special equipment and power consumption height, therefore said method is all not suitable for large-scale production and industrialization.
The present inventor discloses a kind of employing POSS base hydridization fluoroacrylic resin system in patent CN103435741A
For obtaining being applicable to the film of oil-water separation, although this film can be used for removing the micro-moisture in fuel oil, but this resin is in system
Standby process needs to introduce a certain amount of fluorochemical monomer to increase hydrophobicity, cost and pollute the biggest.To this end, the present inventor
Patent application CN105131780A discloses a kind of block propylene acid ester copolymer containing POSS utilizing free-floride and passes through spraying process
Prepare super-hydrophobic coat, although the method does not use fluorochemical monomer in preparation process, but this contains POSS block third
Olefin(e) acid ester copolymer is prepared by Transfer Radical Polymerization (ATRP), and the method needs relatively in building-up process
For exacting terms, needing the environment of complete anaerobic, the film lipophile simultaneously prepared is the best, and then cannot give birth on a large scale
Produce and directly apply to oil-water separation field, it is therefore desirable to the method being improved research and allows it to realize extensive life
Produce, be preferably applied for oil-water separation field.
Summary of the invention
The shortcoming and defect existed for existing super-hydrophobic/super-oleophilic material, the present invention provides and need not use costliness
Fluorine-containing material, raw material is easy to get, and synthesis and spraying coating process are simple, it is easy to being coated with based on POSS base hydridization acrylate of large-scale production
Super-hydrophobic/super-oleophilic stainless (steel) wire of layer and preparation method thereof.
The present invention also aims to provide described super-hydrophobic/super-oleophilic stainless (steel) wire answering in industry oil-water separation
With.
The purpose of the present invention is achieved through the following technical solutions:
A kind of super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings and preparation method thereof, bag
Include following steps:
1) 50～1000 mesh stainless (steel) wires are used respectively dilute hydrochloric acid, dehydrated alcohol and deionized water ultrasonic cleaning, and use nitrogen
Air-blowing is done standby；
2) by POSS base hydridization acrylate polymer ultrasonic dissolution, in ethyl acetate or oxolane or the two is mixed
In bonding solvent, obtain the polymer solution that mass fraction is 1～15%；In terms of mass fraction, described POSS base hydridization propylene
In acid ester polymer, POSS monomer accounts for 5～30%, and methyl methacrylate monomer accounts for 40～65%, acrylic acid higher alkyl esters or
High alkyl methacrylates monomer accounts for 2～20%；
Described POSS monomer structure formula is:
Wherein R is CH3, CH2CH3Or CH2CH(CH3)CH3；R ' is (CH2)nOOCC(CH3)CH2, n be 2～6 whole
Number；
3) at temperature is 25～30 DEG C, the firming agent accounting for liquid quality fraction 0.5～5% is joined step 2) in institute
Polymer solution in, quickly mixing and the most immediately employing spray gun spraying to step 1) in the stainless (steel) wire surface of gained, to obtain final product
To super-hydrophobic/super-oleophilic stainless (steel) wire.
For realizing the object of the invention further, it is preferable that described POSS base hydridization acrylate is molten by free radical
The method of liquid polymerization prepares, and concrete preparation process is as follows: using dimethylbenzene/butyl acetate as reaction dissolvent, azo two is different
Butyronitrile, as initiator, first will account for the 40 of solvent quality～the solvent of 60% joins in reactor and at 80～85 DEG C next time
Stream 20～50min, then by methyl methacrylate, POSS monomer, acrylic acid higher alkyl esters or the senior alkane of methacrylic acid
Base ester monomer, initiator and residual solvent mix homogeneously, be at the uniform velocity added drop-wise in reactor in 2h under nitrogen protection, drips off follow-up
Continuous reaction 4～6h, cooling discharge, at 80 DEG C, solvent is evaporated and obtains POSS base hydridization acrylate polymer.
Preferably, described acrylic acid higher alkyl esters monomer is dodecylacrylate, aliphatic acrylate,
Octadecyl acrylate or octadecyl methacrylate.
Preferably, described stainless (steel) wire is 302 stainless (steel) wires, 304 stainless (steel) wires, 304L stainless (steel) wire, 316 rustless steels
Any one in net, 316L stainless (steel) wire；Described stainless (steel) wire sizing grid is 50～1000 mesh.
Preferably, dilute hydrochloric acid concentration is 1～4mol L‐1；The time of described ultrasonic cleaning is respectively 10～15min；Institute
The time stating ultrasonic dissolution is 5～30min.
Preferably, described firming agent is cyanacrylate, BCA or alpha-cyanoacrylate positive penta
One in ester.
Preferably, described pressure when using spray gun spraying is 0.2～0.4MPa, and spray distance is 5～15cm, nozzle
A diameter of 0.5～5mm.
A kind of super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings, is prepared by said method.
Stainless (steel) wire surface spraying of the present invention forms the polymer spheroids thing with binary micro nano structure, at sky
In gas, the contact angle of water is more than 150 °, and the contact angle of oil, less than 10 °, has super-hydrophobic/super-oleophilic, can be applicable to industry profit
The separation of mixture.
The application in industry oil aqueous mixtures separates of the described super-hydrophobic/super-oleophilic stainless (steel) wire.Described oil mixing with water
Grease separation in thing descends at least one freely: normal hexane, isobutyltrimethylmethane., petroleum ether, vegetable oil and kerosene.
The invention mechanism of above-mentioned super-hydrophobic/super-oleophilic stainless (steel) wire: POSS base hydridization acrylate polymer is selected
Solvent in can form substantial amounts of micelle, this mixed solution is through spraying in substrate, along with the volatilization of solvent, between micelle constantly
Assemble formation spherical, and then define rough surface；Still further aspect, owing in polymer, POSS unit has what table was assembled
R base in ability, and POSS unit is alkane chain, has hydrophobicity, and then reduces coating surface free energy, is polymerized simultaneously
In thing, acrylic acid higher alkyl esters has provided preferably lipophile and certain hydrophobicity, hence in so that the rustless steel prepared
Net has super-hydrophobic/super-oleophilic characteristic.
The present invention compared with prior art, has the advantage that
1) the super-hydrophobic/super-oleophilic stainless (steel) wire preparation process obtained by the present invention is simple, it is not necessary to use fluorine-containing material,
Used material is easy to get, with low cost, and synthesis and spraying coating process are simple, can room temperature fast-curing, and then extensive work can be realized
Industry metaplasia is produced.
2) present invention prepares POSS base hydridization acrylate polymer by the method for solution free radical polymerization, and the method is closed
One-tenth condition is simple, only can need to react after simply leading to nitrogen deoxygenation, it is not necessary to require the environment of complete anaerobic, overcomes existing
The technology CN105131780A preparation method containing POSS block propylene acid ester copolymer super-hydrophobic coat is had to need complete anaerobic
The requirement of environment.
3) present invention introduces the acrylic acid higher alkyl esters monomer of long-chain in this polymer and substantially increases film
Lipophile, therefore by this polymer film stainless (steel) wire of preparing of spraying, there is preferable hydrophobic oleophilic oil characteristic, permissible
Realize the efficient sharp separation to normal hexane, isobutyltrimethylmethane., petroleum ether, vegetable oil and kerosene etc., simultaneously this nethike embrane environment-protecting asepsis evil,
Can be recycled, there is preferable stability；Preferably overcome prior art CN105131780A containing the acid of POSS block propylene
The problem that film lipophile that ester copolymer super-hydrophobic coat obtains is the best.
Accompanying drawing explanation
Fig. 1 a is scanning electron microscope (SEM) figure of 300 mesh stainless (steel) wires the most cleaned in embodiment 1, and amplification is 200
Times；
Fig. 1 b is scanning electron microscope (SEM) figure of the super-hydrophobic/super-oleophilic stainless (steel) wire of embodiment 1 preparation, and amplification is
200 times；
Fig. 1 c and partial enlargement scanning electron microscope (SEM) figure that Fig. 1 d is this super-hydrophobic/super-oleophilic stainless (steel) wire, amplification
It is respectively 1000 times and 5000 times；
Fig. 2 a is the super-hydrophobic/super-oleophilic stainless (steel) wire of the embodiment 1 preparation contact angle photo to deionized water；
Fig. 2 b is this stainless (steel) wire of the embodiment 1 contact angle photo to normal hexane；
Fig. 3 a is the super-hydrophobic/super-oleophilic stainless (steel) wire of the embodiment 1 preparation oil-water separation efficiency chart to different oil；
Fig. 3 b is the repeated isolation conventional efficient figure of embodiment 1 stainless (steel) wire.
Detailed description of the invention
For being best understood from the present invention, below in conjunction with embodiment and accompanying drawing, the present invention will be further described, but this
Bright claimed scope is not limited to the scope represented by embodiment.
Embodiment 1
1) preparation of POSS base hydridization acrylate polymer
Free radical solution polymerization method is used to prepare POSS base hydridization acrylate polymer: first equipped with electric stirring
Machine, constant pressure funnel, N2The four-hole boiling flask of airway and condensing reflux pipe adds 10g dimethylbenzene/butyl acetate (V/V=1/1)
As solvent, it is warming up to 80 DEG C, is stirred at reflux 30min with the speed of 320 revs/min, is passed through N2, then by 8g methacrylic acid
Methyl ester, 2g octadecyl methacrylate, 2.5gPOSS monomer (R=CH2CH(CH3)CH3；N=3), 0.240g azo two
Join constant pressure funnel after isopropyl cyanide and 6.75g dimethylbenzene/butyl acetate (V/V=1/1) mix homogeneously, drip continuously in 2h
Continuing reaction 6h, cooling discharge after complete, the polymer solution finally prepared is dried at 80 DEG C, completely removes solvent, i.e. obtains
POSS base hydridization acrylate polymer.
2) 300 mesh 304 stainless (steel) wires (a size of 3cm × 3cm) are used 1mol L respectively‐1Dilute hydrochloric acid, dehydrated alcohol and go
Ionized water ultrasonic cleaning 10min, and dry up standby with nitrogen；
3) preparation of polymer solution
Taking 1gPOSS base hydridization acrylate in 10g ethyl acetate, ultrasonic 20min makes polymer be completely dissolved, and to obtain final product
It is the polymer solution of 10% to mass fraction；
4) preparation of super-hydrophobic/super-oleophilic stainless (steel) wire
At temperature is 30 DEG C, the cyanacrylate accounting for liquid quality fraction 2% is joined in polymer solution,
Quickly mixing, using nozzle diameter is the spray gun of 1mm, and spray pressure is 0.4MPa, and spray distance is 10cm, by prepare
Mixed solution is sprayed on the stainless (steel) wire of cleaning immediately, i.e. prepares super-hydrophobic/super-oleophilic rustless steel after cold curing 30min
Net.
The present invention spray to polymer solution one step to have prepared on stainless (steel) wire have micro nano structure super-hydrophobic/
Super oleophylic nethike embrane.Fig. 1 a is scanning electron microscope (SEM) figure of the most cleaned 300 mesh stainless (steel) wires of the present invention, and this figure shows, without
The stainless (steel) wire twine smooth surface of spray treatment, Fig. 1 b, Fig. 1 c and Fig. 1 d be the super-hydrophobic/super-oleophilic obtained by the present invention not
The scanning electron microscope (SEM) photograph of rust steel mesh, it can clearly be seen that after spraying, twine surface attachment has and substantial amounts of has the poly-of micro nano structure
Compound microsphere, thus impart the characteristic of stainless (steel) wire super-hydrophobic/super-oleophilic.
Fig. 2 a is the super-hydrophobic/super-oleophilic stainless (steel) wire of the embodiment of the present invention 1 preparation contact angle photo to deionized water,
Fig. 2 b is this stainless (steel) wire contact angle photo to normal hexane, it can be seen that deionized water is at prepared stainless (steel) wire
The contact angle on surface is 153 °, and the normal hexane contact angle on this surface is 0 °, shows that the stainless (steel) wire surface prepared has super thin
Water/super-oleophilic.This defines the polymer microballoon of micro nano structure, this micro-nano knot on twine after being mainly due to spraying
Structure contributes to pinning air, and in this polymer, POSS unit has the ability that table is assembled, and the R base on POSS unit simultaneously
Being alkane chain, have hydrophobicity, and then reduce coating surface free energy, in polymer, acrylic acid higher alkyl esters provides simultaneously
Preferable lipophile and certain hydrophobicity, hence in so that the stainless (steel) wire prepared has super-hydrophobic/super-oleophilic characteristic.
Prepared super-hydrophobic/super-oleophilic stainless (steel) wire net is cut into the circle that radius is 2.5cm, is placed in two fixtures
Between, pinch seal, fixture upper and lower side is all connected to quartz glass tube, and device is disposed vertically, and pours oil-water mixture into, and oil can quickly lead to
Cross stainless (steel) wire, and water can be arrested in the glass tubing of upper end.Fig. 3 a be the embodiment of the present invention 1 preparation super-hydrophobic/super-oleophilic not
The rust steel mesh oil-water separation efficiency to different oil, Fig. 3 b is the repeated isolation experiment of this stainless (steel) wire.Understand from two figures, this
Bright prepared stainless (steel) wire can efficiently and rapidly separate profits such as including normal hexane, isobutyltrimethylmethane., petroleum ether, vegetable oil and diesel oil
Mixture, and can have preferable stability with repeated isolation 25 times, this is mainly due to add in spraying process can
The cyanoacrylate firming agent of cold curing, improves film adhesive force on twine.
Embodiment 2
1) preparation of POSS base hydridization acrylate polymer
Free radical solution polymerization method is used to prepare POSS base hydridization acrylate polymer: first equipped with electric stirring
Machine, constant pressure funnel, N2The four-hole boiling flask of airway and condensing reflux pipe adds 10g dimethylbenzene/butyl acetate (V/V=1/1)
As solvent, it is warming up to 85 DEG C, is stirred at reflux 20min with the speed of 320 revs/min, is passed through N2, then by 9g methacrylic acid
Methyl ester, 2.3g dodecylacrylate, 2.7gPOSS monomer (R=CH2CH3；N=3), 0.280g azodiisobutyronitrile and 8g
Join constant pressure funnel after dimethylbenzene/butyl acetate (V/V=1/1) mix homogeneously, after dripping off continuously in 2h, continue reaction
6h, cooling discharge, the polymer solution finally prepared is dried at 80 DEG C, completely removes solvent, i.e. obtains POSS base hydridization third
Olefine acid ester polymer.
2) 500 mesh 302 stainless (steel) wires (a size of 3cm × 3cm) are used 4mol L respectively‐1Dilute hydrochloric acid, dehydrated alcohol and go
Ionized water ultrasonic cleaning 10min, and dry up standby with nitrogen；
3) preparation of polymer solution
Taking 1gPOSS base hydridization acrylate in 1 5g oxolane, ultrasonic 25min makes polymer be completely dissolved, and to obtain final product
It is the polymer solution of 6.67% to mass fraction；
4) preparation of super-hydrophobic/super-oleophilic stainless (steel) wire
At temperature is 25 DEG C, the alpha-cyanoacrylate n-pentyl ester accounting for liquid quality fraction 0.5% is joined polymer molten
In liquid, quickly mixing, using nozzle diameter is the spray gun of 0.5mm, and spray pressure is 0.3MPa, and spray distance is 15cm, will system
The standby mixed polymer solution obtained is sprayed on the stainless (steel) wire of cleaning immediately, i.e. prepare after cold curing 30min super-hydrophobic/
Super oleophylic stainless (steel) wire.
The present invention spray to polymer solution one step to have prepared on stainless (steel) wire have micro nano structure super-hydrophobic/
Super oleophylic nethike embrane, the deionized water contact angle on prepared stainless (steel) wire surface is 150.1 °, and normal hexane is in the contact on this surface
Angle is 2 °,
Prepared super-hydrophobic/super-oleophilic stainless (steel) wire net is cut into the circle that radius is 2.5cm, is placed in two fixtures
Between, pinch seal, fixture upper and lower side is all connected to quartz glass tube, and device is disposed vertically, and pours oil-water mixture into, and oil can quickly lead to
Cross stainless (steel) wire, and water can be arrested in the glass tubing of upper end.The stainless (steel) wire that the present invention prepares can efficiently and rapidly separate many
Plant oil water mixture, and can carry out separation is repeated several times, there is preferable stability.
Embodiment 3
1) preparation of POSS base hydridization acrylate polymer
Free radical solution polymerization method is used to prepare POSS base hydridization acrylate polymer: first equipped with electric stirring
Machine, constant pressure funnel, N2The four-hole boiling flask of airway and condensing reflux pipe adds 7.5g dimethylbenzene/butyl acetate (V/V=1/1)
As solvent, it is warming up to 80 DEG C, is stirred at reflux 40min with the speed of 320 revs/min, is passed through N2, then by 6g methacrylic acid
Methyl ester, 1.8g octadecyl acrylate, 2gPOSS monomer (R=CH2CH(CH3)CH3；N=6), 0.196g azo two isobutyl
Join constant pressure funnel after nitrile and 5g dimethylbenzene/butyl acetate (V/V=1/1) mix homogeneously, drip off follow-up in 2h continuously
Continuous reaction 4h, cooling discharge, the polymer solution finally prepared is dried at 80 DEG C, completely removes solvent, i.e. obtains POSS base
Hydridization acrylate polymer.
2) 1000 mesh 316L stainless (steel) wires (a size of 3cm × 3cm) are used 2mol L respectively‐1Dilute hydrochloric acid, dehydrated alcohol and
Deionized water ultrasonic cleaning 15min, and dry up standby with nitrogen；
3) preparation of polymer solution
Taking 0.5gPOSS base hydridization acrylate in 25g ethyl acetate, ultrasonic 30min makes polymer be completely dissolved, i.e.
Obtain the polymer solution that mass fraction is 2%；
4) preparation of super-hydrophobic/super-oleophilic stainless (steel) wire
At temperature is 28 DEG C, the BCA accounting for liquid quality fraction 4% is joined polymer solution
In, quickly mix, using nozzle diameter is the spray gun of 1mm, and spray pressure is 0.2MPa, and spray distance is 5cm, will prepare
Mixed polymer solution be sprayed on immediately cleaning stainless (steel) wire on, i.e. prepare super-hydrophobic/super-oleophilic after cold curing 30min
Stainless (steel) wire.
The present invention spray to polymer solution one step to have prepared on stainless (steel) wire have micro nano structure super-hydrophobic/
Super oleophylic nethike embrane, the deionized water contact angle on prepared stainless (steel) wire surface is 152.1 °, and normal hexane is in the contact on this surface
Angle is 1 °,
Prepared super-hydrophobic/super-oleophilic stainless (steel) wire net is cut into the circle that radius is 2.5cm, is placed in two fixtures
Between, pinch seal, fixture upper and lower side is all connected to quartz glass tube, and device is disposed vertically, and pours oil-water mixture into, and oil can quickly lead to
Cross stainless (steel) wire, and water can be arrested in the glass tubing of upper end.The stainless (steel) wire that the present invention prepares can efficiently and rapidly separate many
Plant oil water mixture, and can carry out separation is repeated several times, there is preferable stability.
Claims (10)
1. the preparation method of super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings, it is characterised in that
Comprise the following steps:
1) stainless (steel) wire is used respectively dilute hydrochloric acid, dehydrated alcohol and deionized water ultrasonic cleaning, and dry up with nitrogen standby；
2) by POSS base hydridization acrylate polymer ultrasonic dissolution in ethyl acetate or oxolane or the mixed solvent of the two
In, obtain the polymer solution that mass fraction is 1～15%；In terms of mass fraction, described POSS base hydridization acrylate gathers
In compound, POSS monomer accounts for 5～30 parts, and methyl methacrylate monomer accounts for 40～65 parts, acrylic acid higher alkyl esters or methyl-prop
Olefin(e) acid higher alkyl esters monomer accounts for 2～20 parts；
Described POSS monomer structure formula is:
Wherein R is CH3, CH2CH3Or CH2CH(CH3)CH3；R ' is (CH2)nOOCC(CH3)CH2, n is the integer of 2～6；
3) at temperature is 25～30 DEG C, the firming agent accounting for liquid quality fraction 0.5～5% is joined step 2) in gained
In polymer solution, quickly mixing and the most immediately employing spray gun spraying to step 1) in the stainless (steel) wire surface of gained, i.e. surpassed
Hydrophobic/super oleophylic stainless (steel) wire.
Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings the most according to claim 1
Preparation method, it is characterised in that described POSS base hydridization acrylate is the method system being polymerized as follows by free-atom aqueous solution
For obtaining: using dimethylbenzene/butyl acetate as reaction dissolvent, azodiisobutyronitrile, as initiator, first will account for solvent quality
40～60% solvent join in reactor and at 80～85 DEG C, reflux 20～50min, then by methyl methacrylate
Ester, POSS monomer, acrylic acid higher alkyl esters or high alkyl methacrylates monomer, initiator and residual solvent mixing are all
Even, at the uniform velocity it is added drop-wise in reactor in 2h under nitrogen protection, continuation reaction 4～6h after dripping off, cooling discharge, will at 80 DEG C
Solvent is evaporated and obtains POSS base hydridization acrylate polymer.
Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings the most according to claim 1 and 2
Preparation method, it is characterised in that described acrylic acid higher alkyl esters monomer is dodecylacrylate, acrylic acid 16
Arrcostab, octadecyl acrylate or octadecyl methacrylate.
A kind of super-hydrophobic/super-oleophilic rustless steel based on POSS base hydridization acrylate coatings the most according to claim 1
Net preparation method, it is characterised in that described stainless (steel) wire be 302 stainless (steel) wires, 304 stainless (steel) wires, 304L stainless (steel) wire,
Any one in 316 stainless (steel) wires and 316L stainless (steel) wire；Described stainless (steel) wire sizing grid is 50～1000 mesh.
Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings the most according to claim 1
Preparation method, it is characterised in that described dilute hydrochloric acid concentration is 1～4mol L‐1；The time of described ultrasonic cleaning is respectively
10～15min；The time of described ultrasonic dissolution is 5～30min.
Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings the most according to claim 1
Preparation method, it is characterised in that described firming agent is cyanacrylate, BCA or alpha-cyanoacrylate
One in n-pentyl ester.
Super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings the most according to claim 1
Preparation method, it is characterised in that described pressure when using spray gun spraying is 0.2～0.4MPa, spray distance be 5～
15cm, nozzle diameter is 0.5～5mm.
8. a super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings, it is characterised in that it is by weighing
Profit requires that preparation method described in 1～8 any one prepares；Described stainless (steel) wire surface spraying is formed has binary micro nano structure
Polymer spheroids thing, the contact angle of water is more than 150 ° in atmosphere, and the contact angle of oil less than 10 °, has super-hydrophobic/super-oleophilic
Property.
9. claim 8 super-hydrophobic/super-oleophilic stainless (steel) wire based on POSS base hydridization acrylate coatings is at industry oil moisture
Application in from.
Application the most according to claim 9, it is characterised in that the described grease separation in oil water mixture is from normal hexane, different
In octane, petroleum ether, vegetable oil and kerosene at least one.
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| CN201610756521.9A CN106215462B (en) | 2016-08-29 | 2016-08-29 | Super-hydrophobic/super-oleophilic stainless (steel) wire and the preparation method and application thereof based on POSS base hydridization acrylate coatings |
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| CN201610756521.9A CN106215462B (en) | 2016-08-29 | 2016-08-29 | Super-hydrophobic/super-oleophilic stainless (steel) wire and the preparation method and application thereof based on POSS base hydridization acrylate coatings |
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| CN106215462A true CN106215462A (en) | 2016-12-14 |
| CN106215462B CN106215462B (en) | 2018-09-14 |
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Cited By (6)
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| CN106832157A (en) * | 2017-01-03 | 2017-06-13 | 华南理工大学 | One kind is containing fluorine-containing three block acrylate copolymers of POSS and preparation method thereof |
| CN109248790A (en) * | 2018-10-15 | 2019-01-22 | 四川大学 | Huge surfactant and preparation method thereof for mineral floating |
| CN109289559A (en) * | 2018-10-09 | 2019-02-01 | 西北工业大学 | The preparation method of hydrophobic oleophilic oil self-supported membrane high-molecular porous film and composite hydrophobic oleophylic separation material |
| CN110452490A (en) * | 2019-08-29 | 2019-11-15 | 安徽立兴化工有限公司 | Double POSS polyethers hydridization water-based acrylic resin dispersions, preparation method and the composition for being used to prepare the resin coating film |
| CN115253685A (en) * | 2022-07-11 | 2022-11-01 | 深圳高性能医疗器械国家研究院有限公司 | Janus film and preparation method thereof |
| CN115253685B (en) * | 2022-07-11 | 2024-05-28 | 深圳高性能医疗器械国家研究院有限公司 | Janus membrane and preparation method thereof |
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| CN105131780A (en) * | 2015-08-28 | 2015-12-09 | 华南理工大学 | POSS-block-containing acrylate copolymer super-hydrophobic coating and preparing method thereof |
| CN105418837A (en) * | 2015-12-20 | 2016-03-23 | 华南理工大学 | Preparation method for phase-separation induced porous super-hydrophobic coating material |
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| CN103435742A (en) * | 2013-08-27 | 2013-12-11 | 华南理工大学 | Hydrophobic POSS (Polyhedral Oligomeric Silsesquioxane)-based hybridization fluorinated acrylate resin as well as preparation method and application thereof |
| CN104689602A (en) * | 2015-03-22 | 2015-06-10 | 河北工业大学 | Preparation method of inorganic substance coating oil-water separation mesh |
| CN105131780A (en) * | 2015-08-28 | 2015-12-09 | 华南理工大学 | POSS-block-containing acrylate copolymer super-hydrophobic coating and preparing method thereof |
| CN105418837A (en) * | 2015-12-20 | 2016-03-23 | 华南理工大学 | Preparation method for phase-separation induced porous super-hydrophobic coating material |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106832157A (en) * | 2017-01-03 | 2017-06-13 | 华南理工大学 | One kind is containing fluorine-containing three block acrylate copolymers of POSS and preparation method thereof |
| CN106832157B (en) * | 2017-01-03 | 2019-07-16 | 华南理工大学 | One kind is containing fluorine-containing three block acrylate copolymer of POSS and preparation method thereof |
| CN109289559A (en) * | 2018-10-09 | 2019-02-01 | 西北工业大学 | The preparation method of hydrophobic oleophilic oil self-supported membrane high-molecular porous film and composite hydrophobic oleophylic separation material |
| CN109248790A (en) * | 2018-10-15 | 2019-01-22 | 四川大学 | Huge surfactant and preparation method thereof for mineral floating |
| CN109248790B (en) * | 2018-10-15 | 2019-08-23 | 四川大学 | Huge surfactant and preparation method thereof for mineral floating |
| CN110452490A (en) * | 2019-08-29 | 2019-11-15 | 安徽立兴化工有限公司 | Double POSS polyethers hydridization water-based acrylic resin dispersions, preparation method and the composition for being used to prepare the resin coating film |
| CN110452490B (en) * | 2019-08-29 | 2021-09-17 | 安徽立兴化工有限公司 | Dual POSS polyether hybrid water-based acrylic resin dispersion, preparation method and composition for preparing resin coating film |
| CN115253685A (en) * | 2022-07-11 | 2022-11-01 | 深圳高性能医疗器械国家研究院有限公司 | Janus film and preparation method thereof |
| CN115253685B (en) * | 2022-07-11 | 2024-05-28 | 深圳高性能医疗器械国家研究院有限公司 | Janus membrane and preparation method thereof |
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| CN106215462B (en) | 2018-09-14 |
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