CN107778515B - A kind of short-cut method preparing the super-hydrophobic polycarbonate plate of automatically cleaning yellow - Google Patents
A kind of short-cut method preparing the super-hydrophobic polycarbonate plate of automatically cleaning yellow Download PDFInfo
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Abstract
The present invention discloses a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, which comprises the steps of: (1) cleans polycarbonate plate；(2) polycarbonate plate after cleaning is handled using aqueous solution of nitric acid；(3) polycarbonate plate that washes with water that treated, it is modified then to carry out methyl trichlorosilane, trim,ethylchlorosilane or dimethyldichlorosilane；(4) it is dried overnight after taking out modified polycarbonate plate.The present invention is by simply changing the dip time in nitric acid, by the color of PC substrate from light-yellow tinge to buff (orange), the super-hydrophobic polycarbonate plate of automatically cleaning yellow is prepared, and discloses influence of the MTCS reaction time to configuration of surface and wetability.
Description
Technical field
The present invention relates to the preparations of hydrophobic material.To prepare novel self-cleaning yellow super thin more particularly, to a kind of
The short-cut method of water polycarbonate plate.
Background technique
It naturally is to seek the researcher of problem in science solution in the world maximum " referral centre " herein freely
Ground consulting.A beading or distribution water can be divided into super-hydrophobic or ultra-hydrophilic type respectively on a solid surface.In nature, on lotus leaf
Water droplet is glittering.In ancient times, it is believed that this droplet entirely due to thin layer wax disk(-sc) present on lotus leaf.However,
Barthlott et al. examines display under an electron microscope, and nanoscale wax material is uniform on coarse micro emulsion header structure
Covering, exactly this structure result in the ultra-hydrophobicity of lotus leaf, and it is more than 150 ° that water droplet pearl, which reaches contact angle, and under microvariations
Start to roll down surface.It was noted that lotus flower leaf is green and clean always, because the water polo rolled can eliminate leaf surfaces
Present on any dust.This natural natural cleaning effect is referred to as " lotus leaf effect ".It is interesting that since there are light to spread out
The property specific cycle microstructure with interference effect is penetrated, beautiful Morpho sulkowskyi butterfly's wing shows structure indigo plant
Color and self-cleaning effect.Currently, having carried out the research for showing the non-wetting surface of lotus flower effect.Including non-infiltration mark
Board, colored automatically cleaning window and peephole mirror, goggles, colored printing, surface combine the surface of lotus leaf effect and structural color present
It has been obtained for widely paying close attention to.
Organosilan, especially organotrichlorosilane are for forming from the nanofiber of intertexture to the multiple of nanometer spherical structure
Nano-scale is very helpful.Rollings et al. polymerising ethylene base trichlorosilane in the gas phase, in high aspect ratio
Surface on realize fine and close and variable-length nanofiber.These surfaces are super-hydrophobic.On the other hand, high and mccarthy is
Through deposited monochlorosilane and trichlorosilane by solution on silicon wafer and gas phase, and have studied their wettability.Have
The intensive cylinder being intertwined is presented in interest, the deposit deposited in solution phase methyl trichlorosilane on silicon
Shape Nanofiber Network, water contact angle are higher than 170 °.Water is not observed on this three-dimensional cylinder nanofiber surface
Solidification.Shirgholami and colleague are changed aqueous (super hydrophilic) cotton fabric by being simply immersed in MTCS/ toluene solution
For hydrophobic (super-hydrophobic).They form fine and close nano wire coating using MTCS phenomenon of phase separation on the fabric.In grinding for early stage
In studying carefully, Zimmermann etc. is also vapor-deposited to the nano wire from MTCS, becomes super-hydrophobicity.It is colored super thin
Water surface can be by simply being prepared using various pigment and/or dyestuff.Ogihara et al. passes through spray coated paint nanometer
The suspension of grain, in copper, glass, paper is prepared for recoverable coloured super-hydrophobic coat on line and line.By the class for changing pigment
Type and partial size can easily vary the color of super-hydrophobic coat.Ge et al. is it has been reported that pass through monodisperse fluorided silica
The single step of nano silicon particles sprays to manufacture the unrelated coloured super-hydrophobic film of angle.By changing monodisperse silica nanometer
The size of grain (200,250 and 300nm) adjusts separately the color of super-hydrophobic film for indigo plant, green and brown.Ishizaki and
Sakamoto then passes through n-octadecane base trimethoxy by the way that simply magnesium alloy immersion is maintained in 120 DEG C of ultrapure water
Base silane carries out surface chemical modification, is prepared for having the super-hydrophobic magnesium alloy of the coloring of corrosion resistance and damping capacity.By
Simply change dip time in the ultrapure water of boiling, surface color be easily transferred to from the silver with metallic luster it is orange, it is green
Color and orchid tint.
But the preparation method of above-mentioned hydrophobic material is relatively complicated in the prior art.
Summary of the invention
It is an object of the present invention to provide a kind of novel self-cleaning yellow super-hydrophobic polycarbonate plates of preparing
Short-cut method.
In order to achieve the above objectives, the present invention adopts the following technical solutions:
A kind of short-cut method preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, which is characterized in that including as follows
Step:
(1) polycarbonate plate is cleaned；
(2) polycarbonate plate after cleaning is handled using aqueous solution of nitric acid；
(3) polycarbonate plate that washes with water that treated, then carries out methyl trichlorosilane, trim,ethylchlorosilane or diformazan
Base dichlorosilane is modified；
(4) it is dried overnight after taking out modified polycarbonate plate.
Above-mentioned a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, in step (1): will
Polycarbonate plate is immersed in distilled water, ultrasonic cleaning.
Above-mentioned a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, in step (1): super
Sound scavenging period is 15 minutes.
Above-mentioned a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, in step (2): nitre
The concentration of nitric acid is 1-97wt% in aqueous acid.
Above-mentioned a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, in step (2): clear
Polycarbonate plate after washing is directly immersed in aqueous solution of nitric acid, and soaking time is 1-4 days.
Above-mentioned a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, in step (3): will
Methyl trichlorosilane is dissolved in hexane, is configured to the hexane solution of methyl trichlorosilane；Then the polycarbonate after water being cleaned
Plate is placed in the hexane solution of methyl trichlorosilane.
A kind of above-mentioned short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, methyl trichlorosilane oneself
The volume fraction of methyl trichlorosilane is 10% in alkane solution.
A kind of above-mentioned short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, the poly- carbonic acid after water cleaning
Soaking time of the ester plate in the hexane solution of methyl trichlorosilane is 1-30 minutes.
Above-mentioned a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow, in step (4): dry
Dry temperature is 90 DEG C.
Beneficial effects of the present invention are as follows:
The present invention passes through simple nitric acid treatment and methyl trichlorosilane (MTCS), trim,ethylchlorosilane or dimethyl dichloro
Silane carries out that surface is silylated to develop automatically cleaning yellow super-hydrophobicity polycarbonate, has the characteristics that novelty and easy.
By simply changing the dip time in nitric acid, by the color of PC substrate from light-yellow tinge to buff (orange), and
Disclose influence of the MTCS reaction time to configuration of surface and wetability.
Detailed description of the invention
Specific embodiments of the present invention will be described in further detail with reference to the accompanying drawing.
Fig. 1 synthesizes the detailed step of super-hydrophobic polycarbonate；
The SEM image of Fig. 2 differential responses time MTCS modified nitric acid treatment yellow PC: (a) 1 minute, (b) 5 minutes,
(c) 15 minutes, (d) 30 minutes；
Fig. 3 differential responses time by the MTCS nitric acid treatment yellow PC modified laser microscope image: (a) 1 minute,
(b) 5 minutes, (c) 15 minutes, (d) 30 minutes；
SEM the and LASER MIcrosope image of the naked PC of Fig. 4 differential responses time MTCS modification: (a&b) 30 minutes, (c&
D) 60 minutes；
The XPS spectrum that the reaction time that Fig. 5 passes through the MTCS nitric acid treatment yellow PC modified is 30 minutes；
The XPS spectrum that the reaction time that Fig. 6 passes through MTCS modified nitric acid treatment yellow PC is 30 minutes；
The optical photograph of water droplet on the modified PC of Fig. 7 naked PC, nitric acid treatment PC and MTCS；
The performance test of Fig. 8 super-hydrophobic polycarbonate plate of automatically cleaning yellow prepared by the present invention: (a) self-cleaning effect；(b)
Large volume water droplet；(c) coating drying effect；(d-f) optical photograph of water jets impact test；
Fig. 9 SEM image: (a) blank does not have the PC of nitric acid treatment；(b) 24 hours PC of nitric acid treatment are used；
Figure 10 blank there is no the PC of nitric acid treatment to be modified by MTCS after SEM image (reaction time be 15 minutes).
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further below with reference to preferred embodiments and drawings
It is bright.Similar component is indicated in attached drawing with identical appended drawing reference.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
A kind of 1 short-cut method for preparing the super-hydrophobic polycarbonate plate of novel self-cleaning yellow
1.1 material nitric acid (concentration 69wt%) are purchased from Nanjing of China chemical reagent Co., Ltd.Hexane and methyl trichlorine
Silane (MTCS, purity >=97%) is purchased from Sigma Aldrich, USA.Polycarbonate plate (PC substrate) (ECK, 100UU) is purchased from
SUMITOMO CHEMICAL wood industry Co., Ltd.
The synthesis of the super-hydrophobic polycarbonate of 1.2 yellow
It is cleaned by ultrasonic PC substrate 15 minutes with distilled water first.Clean PC substrate is directly immersed in aqueous solution of nitric acid.
The hydrogen nitrate dipping time is 1~4 day, controls the yellow of PC substrate.It observes that PC substrate is in faint yellow after impregnating 1 day, and impregnates 4 days
PC substrate color becomes buff afterwards.This yellow may be the oxynitride layer due to adsorbing on PC substrate surface.However,
After the two sides for scratching PC substrate energetically, yellow is still complete, and confirmation yellow is transferred to inside PC substrate.This may be due to two
Nitrogen oxide may be diffused into the body region of PC substrate polymer architecture when long-time is impregnated.After being taken out in nitric acid, with big
The distilled water of amount cleans PC substrate.It is put into the hexane for the methyl trichlorosilane (MTCS) that freshly prepared percentage by volume is 10%
In solution.Reaction time was differed from -30 minutes 1 minute, and hexane-MTCS solution is brand-new used in every group of test.Finally, will
These PC substrates are dried overnight at 90 DEG C.Fig. 1 shows the detailed step of the synthesis of super-hydrophobicity polycarbonate.Initial
~89 ° ± 2 ° of water contact angle (WCA) is observed on PC substrate；WCA is down to~63 ° ± 3 ° after nitric acid treatment.By silanization
Processing about 5~30 minutes, water contact angle reaches~155 degree ± 2 degree of stationary value.
1.3 characterizations analyze the surface of coating by field emission scanning electron microscope (FE-SEM) (Hitachi, S-4800)
Form.By the length and diameter of SEM image measurement nanofiber and nanosphere.Use LASER microscope (KEYENCE, VK-
X200 series) assessment coating surface roughness.Scan area is 200 × 200 μm2Coating surface 5 times to obtain average table
The end value of surface roughness.By X X-ray photoelectron spectroscopy X (XPS) (Thermo ESCALAB 250Xi electron spectrometer) into
The chemical analysis of row coating.Use Canon's digital camera (15 series of G) shooting optical photograph.Using contact angle measurement
(Ramehart Instrument Co., USA) obtains water contact angle and slide angle.It drips from micropipettor by film coated surface
The water droplet of about 8 μ L waits 10 seconds to reach equilbrium position.With identical program, water droplet is placed into 6 differences on the coating surface
On position, to obtain the end value of the contact angle of coating surface.In addition, after inclination coating surface (1 ° of measurement inclination every time),
The water droplet of placement starts to roll-off, to obtain specific tilt angle.Nearly 6 operations are taken, with the sliding of each sample of determination
Angle value.
2 results and discussion
It carries out the various reaction time in atmospheric pressure and at room temperature, after simple MTCS modification, in the PC base of nitric acid treatment
Different three dimensional silica nanostructures is observed on plate.
2.1 configurations of surface, surface roughness and water contact angle
Excellent super-hydrophobicity can be obtained by nanofibrous structures, because it provides high surface area/height in length and breadth
Than this is highly useful for forming air pocket.Captured air pocket, which can be minimized, in the fiber structure carries out super-hydrophobic state
Solid-liquid interaction (Cassie-Baxter wetting state).Original PC shows smooth and flat configuration of surface, and 24 is small
When nitric acid treatment PC show the not big variation of surface texture (Fig. 9).We have also investigated under the differential responses time, MTCS
The yellow PC substrate of modified nitric acid treatment.Under lower reaction time (1 minute), short nanofiber is observed on surface
(length~0.5~1 micron), the nano SiO 2 particle that connects of these fibers by diameter less than 250nm are constituted.This
A little short nanofibers were grown for a long time after 5 minutes reaction time, formed the nanofiber for the intertexture that diameter is 150nm.Have
Interest forms nanosphere of the diameter within the scope of 150-500nm after the continuous 15 minutes reaction time in structure, and
After 30 minutes, observe that diameter is the almost uniform silica particle sizes of 500nm on the surface.The mutually separation of MTCS
Result in these three-dimensional surface structures.After contacting with surface hydroxyl, reaction is hydrolyzed to form CH 3-O-Si- in MTCS
(OH) 3 group, and Si-OH group condenses 3 group of hydrophobic-Si-O-Si-CH to be formed Fu Zhe on the coating surface.MTCS's
Continuous hydrolysis and condensation are the main reason for short nanofiber are converted to long nanofiber and nanosphere.When for shorter reaction
Between~1 minute, short nanofiber is formd, with the extension of reaction time, more and more 3 groups of CH3-O-Si- (OH)
Condensation forms the nanofiber of long winding and the nanosphere of connection.From SEM image as can be seen that nanofiber is by interconnected
Small nanosphere is constituted.With the increase in reaction time, nanosphere size increases, the big ruler of the formation of nanofiber due to nanosphere
Very little (~500nm) and be interrupted.However, observing that several nanospheres connected each other (indicate red as shown in Fig. 2 (c) and 2 (d)
Color circle).
Fig. 3 shows the laser microscope image of the MTCS nitric acid treatment yellow PC modified to the differential responses time, reaction
Time is 1min, shows wide gap, surface roughness 106nm.However, for 5 minutes or more reaction time, it is modified
The surface PC shows increasing continuously for the surface roughness of 177,195 and 209nm, and less gap and gap are presented respectively.With
The increase in reaction time, surface roughness is slow but stablizes increased the reason is that the size due to Nano particles of silicon dioxide increases
It is long.With the extension of reaction time, Nano particles of silicon dioxide is largely evenly distributed on the yellow PC of nitric acid treatment.Laser
MIcrosope image matches well with SEM image.
Under the differential responses time, WCA is measured by the nitric acid treatment yellow PC of MTCS modification.When for lower reaction
Between~1 minute, the WCA observed is 143 ° ± 2 °, but water droplet is suspended from surface in any tilt angle.It is such
Wetability can be divided into metastable Cassie-Baxter wetting state, because absorbing relatively high contact angle, water droplet will not be from
Surface tumbles.Due to big gap, sub-fraction water droplet is sandwiched in inside non-uniform surface texture.For 5 minutes to 30 points
The reaction time of clock, WCA keep nearly constant at 155 ° ± 2 °, keep slide angle at 8 ° ± 1 °.These surface classifications are
Stable Cassie-Baxter wetting state.
Observe the homoepitaxial of nano SiO 2 particle and nanofiber on the PC substrate of nitric acid treatment.In order to demonstrate,prove
The specific surface MTCS is modified on the PC substrate of tangible nitric acid treatment, it is intended to MTCS table is carried out in naked/original PC substrate
Face is modified.Exposed PC (being free of nitric acid treatment) is also modified by MTCS, as a result with the PC for the nitric acid treatment modified by MTCS into
Row compares.Observe the comparing result that the surface MTCS is modified on naked PC substrate.Reaction time is~1 minute, 5 minutes and 15 points
Short or long nanofiber is not observed in clock.On the contrary, the Nano particles of silicon dioxide of uneven size is random, big portion
Divide individually and is unevenly distributed over (Figure 10) on the naked PC substrate between them with wide arc gap (gap~1~12 μm).
SEM image (Fig. 4 (a) and 4 (c)) shows even if at 30 minutes and after sixty minutes, nano SiO 2 particle on naked PC substrate
Uneven and random covering.Reaction time.Laser microscope image (Fig. 4 (b) and 4 (d)) is not also shown unevenly and not
Uniform pattern, reaction time are respectively 30 and 60 minutes, and mean roughness is 171 and 187nm.With the MTCS reaction time 30
With the water contact angle on the coating of preparation in 60 minutes.Exposed PC substrate due to its non-uniform form, be shown as 114 ° and
121 °, error amount is ± 15 °.
2.2XPS research
XPS analysis is carried out to study the chemical state of element present on the PC of MTCS modification and form.Fig. 5 is shown
The measure spectrum that reaction time by the nitric acid treatment yellow PC of MTCS modification is 30 minutes.Spectrum shows silicon, oxygen, carbon and nitrogen
Presence.The C1s core stage spectrum of modified PC is as shown in Fig. 6 (a).It was found that the spectrum envelope of the C1s core level of modified PC is broad
And it is asymmetric, several carbon components can be identified by disclosing in modified PC.Especially-(C-C)-and -- (C-H)-,-(O=C-O)
,-(C-O-H)-and R-O-C=energy be respectively 284.2eV, 284.8eV, 285.6eV and 285.9eV.It was found that in modified PC
It is 531.7,532.2 and 533.1eV that the combination of O1s (Fig. 6 (b)), which can be worth, this is attributable to C-O-H, Si-O-C and Si-O-Si
Or C-O-C.Although PC without nitrogen groups, corresponds at the peak that 399.4eV is observed (Fig. 6 (c)) in its structure and is used for table
The N1 of nitro in the pretreated nitric acid in face.For the Si2p of 102.5eV, extensive unimodal (Fig. 6 (d)) is had been obtained for, this
Obviously it can solely be attributed to SiO present in coating matrix2Si-O substance in base net network.The result of acquisition strongly suggests that PC
Surface by organosilan (MTCS) modify.
The wetting of 2.3 coatings and self-cleaning performance pass through the modified naked PC of MTCS, nitric acid to study wettability of the surface
The PC and nitric acid treatment PC of processing measure water contact angle (WCA), as a result as shown in Figure 7.Naked PC substrate shows WCA~89 ° ± 2 °,
And nitric acid treatment PC shows~63 ° ± 3 ° of WCA.The decline for being exposed to WCA after nitric acid speculates that polar functional group introduces on surface,
Surface can increase.However, WCA gradually rises after MTCS functionalization, reach~155 ° ± 2 ° of stationary value, continue 5~
30min.This hydrophobic increase discloses surface and is effectively modified by MTCS.PC substrate is immersed in nitric acid 1 and 4 day,
Color becomes buff from light yellow.After the MTCS surface modification reaction time is 30 minutes, surface shows~155 ° ± 2 °
WCA。
It is investigated other properties of super-hydrophobic yellow PC substrate.If water droplet obtains spherical shape on the surface, from
Surface collection dust granule is easier.Because spherical water droplets can easily collect dust granule when rolling.Super hydrophobic surface
Self-cleaning performance obtained the great attention of industrial enterprise.Spray thin black fine coal at random on super-hydrophobic yellow PC substrate
Ash.After landing and rolling, coal dust is liable to stick on spherical water droplets.Fig. 8 (a) depicts the automatically cleaning of super-hydrophobic yellow PC substrate
Performance, wherein drop is fallen on the surface after collecting dust granule.Mild just giving a puff can be the acquisition of this dust
Water polo rolls down, and keeps surface cleaning.The water polo of 10ml volume is gently placed on (Fig. 8 in super-hydrophobic yellow PC substrate
(b)), because large volume water polo on super hydrophobic surface to roll out probability very high.These water droplets keep stable on the surface
Nearly 10 minutes.The osmosis of surface micro-structure in water is observed at room temperature.However, after being kept for the so long time, gently
Push substrate that can make water lower rolling in the case where surface is not fixed, this shows water not in surface micro-structure internal penetration.
Super hydrophobic surface be substantially it is dry, they will not allow water to leave.By the way that super-hydrophobic yellow PC matrix is placed in training
It supports in ware and pours into water and wherein observe this drying effect (Fig. 8 (c)).Even if culture dish is full, water is not skipped super-hydrophobic yet
The surface of yellow PC substrate.Water forms high about 1 centimetre of water wall in super-hydrophobic yellow PC substratel.Therefore, super-hydrophobic yellow
PC substrate shows the resistance to water in terms of wetability, to confirm its stemness.The durability on super hydrophobic surface is industry
The principal concern of middle daily use.The durability of super-hydrophobic coat is usually surveyed by water droplet or the water jets impact of height
Examination.High velocity water droplets or water jet should be able to damage the final micro/nano structure or coarse structure for influencing surface wettability.Such as Fig. 8
(d-f) shown in, water jet impacts on super-hydrophobic yellow PC substrate (video clipping such as SI in a manner of perpendicular to upright position
It is shown).Vertical water jets impact may damage coating than inclined water jets impact.However, coating does not damage nearly 5 under water slug
Minute.After water jets impact, WCA measurement result is not confirmed.
3 conclusions
Effective automatically cleaning yellow super-hydrophobicity polycarbonate is prepared for by simple nitric acid treatment and MTCS modification.It is logical
Spending the control hydrogen nitrate dipping time simply controls the yellowing degree of PC.On the PC of nitric acid treatment, the reaction time of MTCS is different,
Three-dimensional manometer fiber and nanosphere micro-structure are provided on substrate.These forms are responsible for the excellent super-hydrophobicity on surface and from clearly
Clean performance.On the basis of XPS analysis, due to forming C=O, Si-O-C and Si-O-Si group, the nitric acid being modified by MTCS
The PC of reason shows significant super-hydrophobicity, while producing surface roughness.Our novel easily system prepares self-cleaning
Colored super hydrophobic surface, does not need specific illuminating colour, does not need maintenance clean surface yet.Self-cleaning colour super-hydrophobic surface
Huge market can be seized in decorative applications.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is all to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the scope of protection of the present invention.
Claims (1)
1. a kind of short-cut method for preparing the super-hydrophobic polycarbonate plate of automatically cleaning yellow, which comprises the steps of:
(1) polycarbonate plate is cleaned；Polycarbonate plate is immersed in distilled water, is cleaned by ultrasonic；Being cleaned by ultrasonic the time is 15 points
Clock；
(2) polycarbonate plate after cleaning is handled using aqueous solution of nitric acid；The concentration of nitric acid is 1- in aqueous solution of nitric acid
97wt%；Polycarbonate plate after cleaning is directly immersed in aqueous solution of nitric acid, and soaking time is 1-4 days；
(3) polycarbonate plate that washes with water that treated, then carries out methyl trichlorosilane, trim,ethylchlorosilane or dimethyl two
Chlorosilane is modified；Methyl trichlorosilane is dissolved in hexane, the hexane solution of methyl trichlorosilane is configured to；Then water is cleaned
Polycarbonate plate afterwards is placed in the hexane solution of methyl trichlorosilane；Methyl trichlorosilane in the hexane solution of methyl trichlorosilane
Volume fraction be 10%；Soaking time of the polycarbonate plate in the hexane solution of methyl trichlorosilane after water cleaning is 1-
30 minutes；
(4) it is dried overnight after taking out modified polycarbonate plate；In step (4): drying temperature is 90 DEG C.
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| CN104987528A (en) * | 2015-06-29 | 2015-10-21 | 武汉工程大学 | Modification method of oleophylic and hydrophobic nano-sponge |
| CN105949498A (en) * | 2016-05-19 | 2016-09-21 | 北京林业大学 | Melamine-based sponge for absorbing oil slick and preparation method |
| CN107189656A (en) * | 2017-07-13 | 2017-09-22 | 华北电力大学（保定） | A kind of preparation method of the wear-resisting super-hydrophobic coat based on makrolon |
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