CN106630679B - A method of wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method - Google Patents
A method of wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method Download PDFInfo
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- CN106630679B CN106630679B CN201710016890.9A CN201710016890A CN106630679B CN 106630679 B CN106630679 B CN 106630679B CN 201710016890 A CN201710016890 A CN 201710016890A CN 106630679 B CN106630679 B CN 106630679B
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- 238000000034 method Methods 0.000 title claims abstract description 56
- 230000008961 swelling Effects 0.000 title claims abstract description 27
- 238000000576 coating method Methods 0.000 claims abstract description 115
- 239000011248 coating agent Substances 0.000 claims abstract description 112
- 238000003618 dip coating Methods 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims description 48
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 40
- 239000000853 adhesive Substances 0.000 claims description 39
- 230000001070 adhesive effect Effects 0.000 claims description 39
- 239000004677 Nylon Substances 0.000 claims description 36
- 229920001778 nylon Polymers 0.000 claims description 36
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 20
- 235000019253 formic acid Nutrition 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 16
- 238000004026 adhesive bonding Methods 0.000 claims description 12
- 238000007654 immersion Methods 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- 229910052681 coesite Inorganic materials 0.000 claims description 7
- 229910052906 cristobalite Inorganic materials 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000002791 soaking Methods 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 229910052682 stishovite Inorganic materials 0.000 claims description 7
- 229910052905 tridymite Inorganic materials 0.000 claims description 7
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 4
- 229920000647 polyepoxide Polymers 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920002292 Nylon 6 Polymers 0.000 claims description 3
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Inorganic materials [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 229920003189 Nylon 4,6 Polymers 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229920005749 polyurethane resin Polymers 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 14
- 238000005516 engineering process Methods 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 44
- 239000011521 glass Substances 0.000 description 25
- 239000003921 oil Substances 0.000 description 18
- 238000012545 processing Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 11
- 239000003292 glue Substances 0.000 description 9
- 238000005507 spraying Methods 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 244000137852 Petrea volubilis Species 0.000 description 7
- 238000005299 abrasion Methods 0.000 description 7
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011236 particulate material Substances 0.000 description 4
- 230000035939 shock Effects 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 239000012790 adhesive layer Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000017 hydrogel Substances 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 230000005660 hydrophilic surface Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000010954 inorganic particle Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229960002668 sodium chloride Drugs 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 1
- PXFBZOLANLWPMH-UHFFFAOYSA-N 16-Epiaffinine Natural products C1C(C2=CC=CC=C2N2)=C2C(=O)CC2C(=CC)CN(C)C1C2CO PXFBZOLANLWPMH-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000003486 chemical etching Methods 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000010041 electrostatic spinning Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000004807 localization Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/38—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal at least one coating being a coating of an organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/18—Processes for applying liquids or other fluent materials performed by dipping
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2401/00—Form of the coating product, e.g. solution, water dispersion, powders or the like
- B05D2401/10—Organic solvent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D2505/00—Polyamides
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
A method of wear-resisting super hydrophilic underwater superoleophobic surface being prepared based on swelling method, the present invention relates to a kind of preparation methods of wear-resisting super hydrophilic underwater super oleophobic coating.It is cumbersome the invention solves existing super hydrophilic underwater superoleophobic surface preparation technology and the problem of wear no resistance.Method: one, inorganic particulate coating is prepared；Two, glue-line is sprayed；Three, dip-coating inorganic particulate coating, that is, the method for completing to prepare wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method.The present invention is for a kind of method for preparing wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method.
Description
Technical field
The present invention relates to a kind of preparation methods of wear-resisting super hydrophilic underwater super oleophobic coating.
Background technique
Ultra-hydrophilic surface due to antifog, automatically cleaning, enhancing the fields such as boiling heat transfer and water-oil separating have important application,
It is synthesized extensively in recent years and is applied to different substrate materials.For most of ultra-hydrophilic surfaces, since surface is to the strong affine of water
Power also shows that height oleophobic or superoleophobic characteristic under water.However, the method that tradition prepares ultra-hydrophilic surface is adopted mostly
With surface chemical modification or in the hydrophilic material of surface deposition bad mechanical strength.For example it is published in Advanced Materials
The 23rd phase of the upper 2011 year article of page 4270 " A novel superhydrophilic and underwater
Superoleophobic hydrogel-coated mesh for oil/water separation " describe it is a kind of super close
The preparation method of water superoleophobic stainless (steel) wire under water, by the way that hydrophilic hydrogel to be wrapped on stainless (steel) wire, to make not
The steel mesh that becomes rusty obtains super hydrophilic underwater superoleophobic property, and is applied to water-oil separating, but hydrogel mechanical strength used is poor,
It expands and softens after water suction, be not suitable for large-scale application.It was published in Advanced Materials upper 25th phase in 2013
Article " the Nanowire-haired inorganic membranes with superhydrophilicity and of page 4192
underwater ultralow adhesive superoleophobicity for high-efficiency oil/water
Separation " nanowire etched on copper mesh using the method for chemical etching, to obtain super hydrophilic underwater superoleophobic
Copper mesh can be used for separating emulsion oil-in-water, though not inquiring into the mechanical strength of copper mesh in text, copper mesh is micro- from text
It is still limited to see its mechanical strength known in structure, biggish external force abrasion cannot be born.Other technologies such as electrostatic spinning, electricity
Not only preparation process is cumbersome for chemical polymerization, corona treatment and template etc., but also is difficult to obtain wear-resisting ultra-hydrophilic surface.
Therefore, seek simply, the super hydrophilic underwater superoleophobic surface that pervasive method prepares highly abrasion-resistant is still difficult to realize at present.
Summary of the invention
It is cumbersome the invention solves existing super hydrophilic underwater superoleophobic surface preparation technology and the problem of wear no resistance, and
A kind of method preparing wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method is provided.
A kind of method preparing wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method is completed by the following steps:
One, inorganic particulate coating is prepared:
The formic acid that nylon, hydrophilic inorganic particulate and mass percent are 88% is mixed, obtains applying containing inorganic particulate
Material；
The mass ratio of the nylon and hydrophilic inorganic particulate is 1:(0.5~20)；Described applies containing inorganic particulate
The gross mass percentage of nylon and hydrophilic inorganic particulate is 10%~55% in material；
Two, glue-line is sprayed:
By adhesive even application in substrate surface, uniform glue-line is obtained, then drying is fully cured to glue-line, obtains
The substrate of gluing；
The adhesive is the adhesive that can be swollen by formic acid or can be by the polymer of formic acid swelling；
Three, dip-coating inorganic particulate coating:
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soaking time is 5s~2h, after then impregnating
Substrate extraction is lifted from coating containing inorganic particulate with the speed of 1mm/s~10mm/s, obtain the substrate for being adsorbed with coating, will
It is dry in 20 DEG C~80 DEG C baking ovens that the substrate for being adsorbed with coating, which is placed in temperature, until solvent volatilizees completely, that is, is completed based on molten
The method that swollen method prepares wear-resisting super hydrophilic underwater superoleophobic surface.
The beneficial effects of the present invention are:
1, method of the invention is simple, is not required to by complicated equipment, and raw material is easy to get, and time-consuming short, reaction condition is mild, poison
Property is small.
2, prepared wear-resisting super hydrophilic underwater super oleophobic coating has super hydrophilic underwater superoleophobic characteristic: coating is in air
In be 0 ° to the contact angle of water, 150 ° are greater than to the contact angle of oil under water, slide angle is less than 10 °.
3, prepared wear-resisting super hydrophilic underwater super oleophobic coating has excellent mechanical stability.This method is prepared resistance to
The defect that super hydrophilic underwater superoleophobic surface overcomes the super-hydrophilic coating mechanical stability difference prepared in the past is ground, is substantially increased
It the mechanical life of coating, is with a wide range of applications.
The mechanical stability of coating depends on two aspects: first is that the bond strength of coating and substrate, second is that coating itself
Mechanical strength.
Nylon has good mechanical strength, hardness, dimensional stability, toughness and wearability, thus is used to improve and apply
The performance of layer.The hydroxyl (- OH) of amido bond (- CO-NH-) and hydrophilic surface of inorganic particles in nylon generates strong hydrogen bond
Effect, so that the particle in coating be made firmly to be bonded together, and improves the mechanical strength of coating.In addition, coating sheet
Also there is very strong binding force between body and substrate, this binding force is entangled derived from nylon molecules chain and the physics of adhesive molecule interchain
Twine effect: when the substrate for being coated with adhesive is immersed in coating containing inorganic particulate, formic acid causes adhesive swelling of paint coating, makes
The gap obtained between adhesive strand is gradually increased.The increase of molecule interchain voids allows nylon molecules to take this opportunity to penetrate into
In these gaps, and irregular intertexture occurs with adhesive strand.After formic acid volatilizees completely, nylon molecules and adhesive
It is intermolecular just to form physical entanglement, to obtain high bond strength.The mechanical strength of coating itself and its between substrate
High adhesion strength allows prepared coating to resist complicated mechanical damage.
In addition to this, since coating also has certain thickness and continuous coarse structure, when surface is worn, by
The coating shedding of damage and the coating for exposing junior, the coating exposed has and the consistent roughness of original coating surface, because
And coating can be subjected to abrasion repeatedly and maintain underwater superoleophobic property.
Detailed description of the invention
Fig. 1 is the SEM figure that the substrate surface of gluing in one step 2 of embodiment amplifies 8000 times；
Fig. 2 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one amplifies 2500 times of SEM figure；
Fig. 3 is that 400 times of SEM figure is amplified in wear-resisting super hydrophilic underwater superoleophobic glass slide cross section prepared by embodiment one；
Fig. 4 is that 5000 times of SEM figure is amplified in wear-resisting super hydrophilic underwater superoleophobic glass slide cross section prepared by embodiment one,
1 is adhesive；
Fig. 5 is the contact angle for the wear-resisting super hydrophilic underwater superoleophobic slide surface that water droplet is prepared in embodiment one；
Fig. 6 is the underwater contact angle for the wear-resisting super hydrophilic underwater superoleophobic slide surface that oil droplet is prepared in embodiment one；
Fig. 7 is the prior glass slide without glue spraying processing and the reality with water wetting prepared by the comparative test one soaked with water
The photo of the wear-resisting super hydrophilic underwater superoleophobic glass slide of the preparation of example one is applied, A is the prior without glue spraying of the preparation of comparative test one
The glass slide of processing, B are wear-resisting super hydrophilic underwater superoleophobic glass slide prepared by embodiment one；
Fig. 8 is the prior glass slide without glue spraying processing and the reality with water wetting prepared by the comparative test one soaked with water
The wear-resisting super hydrophilic underwater superoleophobic slide surface of the preparation of example one is applied in the photo after finger friction, A is comparative test
The prior glass slide without glue spraying processing of one preparation, B are wear-resisting super hydrophilic underwater superoleophobic glass slide prepared by embodiment one；
Fig. 9 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one is passing through 24kPa pressure and 600
The contact angle and slide angle of underwater oil when mesh Sandpapering different distance change, and 1 is contact angle, and 2 be slide angle；
Figure 10 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by the embodiment one being spontaneously wet out by water is being passed through
The contact angle and slide angle of underwater oil when 24kPa pressure and 600 mesh Sandpapering different distance change, and 1 is contact angle, and 2 are
Slide angle；
Figure 11 is wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one by flow velocity 3.5m/s and straight
The water column of diameter 5mm washes away the photo after 1h, and 1 is water column shock zone；
The intersection of wear-resisting super hydrophilic underwater super oleophobic coating and adhesive layer that Figure 12 is prepared for embodiment one is through overcurrent
The water column of fast 3.5m/s and diameter 5mm wash away the photo after 1h, and 1 is water column shock zone；
Figure 13 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one is passing through different physics and change
The contact angle and slide angle of underwater oil after learning environmental treatment, " ■ " are contact angle, and " ◆ " is slide angle, and it is -30 that a, which is in temperature,
DEG C air in handle 72h；B is to handle 72h in the air that temperature is 100 DEG C；C is in the deionized water that temperature is 80 DEG C
Processing 12 hours；D is to handle 72h in the aqueous sulfuric acid of pH=1；E is the sodium-chloride water solution that mass percent is 3.5%
Middle processing 72h；F is soak at room temperature 72h in toluene；G is soak at room temperature 72h in ethyl alcohol.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of to prepare wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method
Method is completed by the following steps:
One, inorganic particulate coating is prepared:
The formic acid that nylon, hydrophilic inorganic particulate and mass percent are 88% is mixed, obtains applying containing inorganic particulate
Material；
The mass ratio of the nylon and hydrophilic inorganic particulate is 1:(0.5~20)；Described applies containing inorganic particulate
The gross mass percentage of nylon and hydrophilic inorganic particulate is 10%~55% in material；
Two, glue-line is sprayed:
By adhesive even application in substrate surface, uniform glue-line is obtained, then drying is fully cured to glue-line, obtains
The substrate of gluing；
The adhesive is the adhesive that can be swollen by formic acid or can be by the polymer of formic acid swelling；
Three, dip-coating inorganic particulate coating:
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soaking time is 5s~2h, after then impregnating
Substrate extraction is lifted from coating containing inorganic particulate with the speed of 1mm/s~10mm/s, obtain the substrate for being adsorbed with coating, will
It is dry in 20 DEG C~80 DEG C baking ovens that the substrate for being adsorbed with coating, which is placed in temperature, until solvent volatilizees completely, that is, is completed based on molten
The method that swollen method prepares wear-resisting super hydrophilic underwater superoleophobic surface.
The beneficial effect of present embodiment is: 1, the method for present embodiment is simple, is not required to by complicated equipment, raw material
It is easy to get, time-consuming short, reaction condition is mild, small toxicity.
2, prepared wear-resisting super hydrophilic underwater super oleophobic coating has super hydrophilic underwater superoleophobic characteristic: coating is in air
In be 0 ° to the contact angle of water, 150 ° are greater than to the contact angle of oil under water, slide angle is less than 10 °.
3, prepared wear-resisting super hydrophilic underwater super oleophobic coating has excellent mechanical stability.This method is prepared resistance to
The defect that super hydrophilic underwater superoleophobic surface overcomes the super-hydrophilic coating mechanical stability difference prepared in the past is ground, is substantially increased
It the mechanical life of coating, is with a wide range of applications.
The mechanical stability of coating depends on two aspects: first is that the bond strength of coating and substrate, second is that coating itself
Mechanical strength.
Nylon has good mechanical strength, hardness, dimensional stability, toughness and wearability, thus is used to improve and apply
The performance of layer.The hydroxyl (- OH) of amido bond (- CO-NH-) and hydrophilic surface of inorganic particles in nylon generates strong hydrogen bond
Effect, so that the particle in coating be made firmly to be bonded together, and improves the mechanical strength of coating.In addition, coating sheet
Also there is very strong binding force between body and substrate, this binding force is entangled derived from nylon molecules chain and the physics of adhesive molecule interchain
Twine effect: when the substrate for being coated with adhesive is immersed in coating containing inorganic particulate, formic acid causes adhesive swelling of paint coating, makes
The gap obtained between adhesive strand is gradually increased.The increase of molecule interchain voids allows nylon molecules to take this opportunity to penetrate into
In these gaps, and irregular intertexture occurs with adhesive strand.After formic acid volatilizees completely, nylon molecules and adhesive
It is intermolecular just to form physical entanglement, to obtain high bond strength.The mechanical strength of coating itself and its between substrate
High adhesion strength allows prepared coating to resist complicated mechanical damage.
In addition to this, since coating also has certain thickness and continuous coarse structure, when surface is worn, by
The coating shedding of damage and the coating for exposing junior, the coating exposed has and the consistent roughness of original coating surface, because
And coating can be subjected to abrasion repeatedly and maintain underwater superoleophobic property.
Specific embodiment 2: the present embodiment is different from the first embodiment in that: it is described in step 1 hydrophilic
Property inorganic particulate be SiO2Particle, TiO2Particle or BaSO4Particle.It is other same as the specific embodiment one.
Specific embodiment 3: unlike one of present embodiment and specific embodiment one or two: institute in step 1
The nylon stated is nylon 6,6, nylon 6 or nylon 4,6.It is other the same as one or two specific embodiments.
Specific embodiment 4: unlike one of present embodiment and specific embodiment one to three: institute in step 2
The substrate stated is acid resisting material.It is other identical as specific embodiment one to three.
Specific embodiment 5: unlike one of present embodiment and specific embodiment one to four: institute in step 2
The adhesive stated is adhesive for polyurethane or epoxy resin.It is other identical as specific embodiment one to four.
Specific embodiment 6: unlike one of present embodiment and specific embodiment one to five: institute in step 1
The mass ratio of the nylon and hydrophilic inorganic particulate stated is 1:4.4.It is other identical as specific embodiment one to five.
Specific embodiment 7: unlike one of present embodiment and specific embodiment one to six: institute in step 1
The gross mass percentage of nylon and hydrophilic inorganic particulate is 35% in the coating containing inorganic particulate stated.Other and specific implementation
Mode one to six is identical.
Specific embodiment 8: unlike one of present embodiment and specific embodiment one to seven: will in step 3
The substrate vertical immersion of gluing is in coating containing inorganic particulate, soaking time 10min.Other and specific embodiment one to seven
It is identical.
Specific embodiment 9: unlike one of present embodiment and specific embodiment one to eight: in step 3 so
The substrate after immersion is lifted into extraction with the speed of 2mm/s from coating containing inorganic particulate afterwards.Other and specific embodiment one
It is identical to eight.
Specific embodiment 10: unlike one of present embodiment and specific embodiment one to nine: will in step 3
It is drying in 25 DEG C of baking ovens that the substrate for being adsorbed with coating, which is placed in temperature, until solvent volatilizees completely.Other and specific embodiment
One to nine is identical.
Beneficial effects of the present invention are verified using following embodiment:
Embodiment one:
A kind of method preparing wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method is completed by the following steps:
One, inorganic particulate coating is prepared:
The formic acid that nylon, hydrophilic inorganic particulate and mass percent are 88% is mixed, obtains applying containing inorganic particulate
Material；
The mass ratio of the nylon and hydrophilic inorganic particulate is 1:4.4；Buddhist nun in the coating containing inorganic particulate
The gross mass percentage of imperial and hydrophilic inorganic particulate is 35%；
The nylon is nylon 6,6；The hydrophilic inorganic particulate is SiO2Particle；
Two, glue-line is sprayed:
By adhesive even application in substrate surface, uniform glue-line is obtained, is then dried, until glue-line is fully cured,
Obtain the substrate of gluing；
The adhesive is commercially available 92 epoxy three-proofing coating of Ao Sibang；The substrate is glass slide；
Three, dip-coating inorganic particulate coating:
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soaking time 10min then will be after immersion
Substrate lifts extraction with the speed of 2mm/s from coating containing inorganic particulate, obtains the substrate for being adsorbed with coating, will be adsorbed with coating
Substrate to be placed in temperature be dry in 25 DEG C of baking ovens, until solvent volatilizees completely, obtain wear-resisting super hydrophilic underwater superoleophobic load glass
Piece.
Comparative test one:
One, inorganic particulate coating is prepared:
The formic acid that nylon, hydrophilic inorganic particulate and mass percent are 88% is mixed, obtains applying containing inorganic particulate
Material；
The mass ratio of the nylon and hydrophilic inorganic particulate is 1:4.4；Buddhist nun in the coating containing inorganic particulate
The gross mass percentage of imperial and hydrophilic inorganic particulate is 35%；
The nylon is nylon 6,6；The hydrophilic inorganic particulate is SiO2Particle；
Two, dip-coating inorganic particulate coating:
By substrate vertical immersion in coating containing inorganic particulate, soaking time 10min, then by the substrate after immersion with
The speed of 2mm/s lifts extraction from coating containing inorganic particulate, obtains the substrate for being adsorbed with coating, will be adsorbed with the substrate of coating
It is dry in 25 DEG C of baking ovens for being placed in temperature, until solvent volatilizees completely, obtains the glass slide in advance without glue spraying processing；
The substrate is glass slide.
Fig. 1 is the SEM figure that the substrate surface of gluing in one step 2 of embodiment amplifies 8000 times；As seen from the figure, after solidification
Adhesive coating it is very smooth, without apparent roughness.
Fig. 2 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one amplifies 2500 times of SEM figure；By
Scheme it is found that prepared wear-resisting super hydrophilic underwater superoleophobic surface is by micron-sized SiO2Particle and smaller nylon crystal grain group
At showing very coarse structure.
Fig. 3 is that 400 times of SEM figure is amplified in wear-resisting super hydrophilic underwater superoleophobic glass slide cross section prepared by embodiment one；
As seen from the figure, the particle structure continuously accumulated is presented in prepared wear-resisting super hydrophilic underwater super oleophobic coating, this to work as coating
When being worn, the coating that junior exposes still keeps roughness similar with initial surface, to make the super wetability on surface
It is maintained.
Fig. 4 is that 5000 times of SEM figure is amplified in wear-resisting super hydrophilic underwater superoleophobic glass slide cross section prepared by embodiment one,
1 is adhesive；As seen from the figure, it is shown that wear-resisting super hydrophilic underwater super oleophobic coating, adhesive layer and the friendship of glass slide three
Interface.
Fig. 5 is the contact angle for the wear-resisting super hydrophilic underwater superoleophobic slide surface that water droplet is prepared in embodiment one；By scheming
It is found that intimate 0 ° of contact angle is presented on prepared wear-resisting super hydrophilic underwater superoleophobic surface in water droplet, it was demonstrated that its Superhydrophilic.
Fig. 6 is the underwater contact angle for the wear-resisting super hydrophilic underwater superoleophobic slide surface that oil droplet is prepared in embodiment one；
The oil droplet is 1,2- dichloroethanes；As seen from the figure, underwater oil droplet is in prepared wear-resisting super hydrophilic underwater superoleophobic table
The contact angle greater than 150 ° is presented in face, it was demonstrated that its underwater superoleophobic property.
Fig. 7 is the prior glass slide without glue spraying processing and the reality with water wetting prepared by the comparative test one soaked with water
The photo of the wear-resisting super hydrophilic underwater superoleophobic glass slide of the preparation of example one is applied, A is the prior without glue spraying of the preparation of comparative test one
The glass slide of processing, B are wear-resisting super hydrophilic underwater superoleophobic glass slide prepared by embodiment one；Fig. 8 is the comparison soaked with water
The prior glass slide handled without glue spraying and prepared with the embodiment one that water soaks wear-resisting super hydrophilic underwater prepared by test one
For superoleophobic slide surface in the photo after finger friction, A is the prior without glue spraying processing of the preparation of comparative test one
Glass slide, B are wear-resisting super hydrophilic underwater superoleophobic glass slide prepared by embodiment one；Control is phase as far as possible during finger friction
Same dynamics can be resisted using the wear-resisting super hydrophilic underwater super oleophobic coating that adhesive is fixed well as seen from the figure
Finger friction, and easily worn by finger after being spontaneously wet out by water without the fixed coating of adhesive, thus make coating shedding, this card
Important function of the adhesive in terms of maintaining coating stable is illustrated.
Prepared by the wear-resisting super hydrophilic underwater superoleophobic glass slide prepared to embodiment one and the embodiment one being spontaneously wet out by water
Wear-resisting super hydrophilic underwater superoleophobic slide surface carries out sand paper wear testing；It specifically carries out: will implement according to the following steps
Wear-resisting super hydrophilic superoleophobic glass slide under water and the embodiment one being spontaneously wet out by water prepared by example one prepares wear-resisting super hydrophilic underwater
Superoleophobic slide surface is fixed on desktop (coating is upward), keeps its immovable, the bar shaped sand paper for being 1cm by width
Sand face paste on fixed wear-resisting super hydrophilic underwater superoleophobic surface, and in applying 215g weight on sand paper another side, and
Weight is fixed, is constituted friction system (being from top to bottom followed successively by weight, sand paper, wear-resisting super hydrophilic underwater super oleophobic coating).Line
Property horizontal pulling sand paper make it that opposite sliding occur in a localization (1cm × 0.9cm) of ultra-hydrophilic surface (to pull by hand i.e.
Can, drawing velocity influences less, to can be ignored on experimental result), to generate abrasion to surface.Due to sand paper limited length, often
It is secondary to pull 10cm as standard, (1cm × 0.9cm) carries out repeated multiple times pull in identical region.Experimental result is to wear
The contact angle of the underwater oil in region and the variation characterization of slide angle relative wear distance, every friction 10cm measurement eroded area are underwater
The contact angle and slide angle of oil.Pressure then according to apply weight weight 215g and eroded area (1cm × 0.9cm) area into
Row conversion show that pressure is 24kPa.The sand paper is 600 mesh.Test result is as shown in FIG. 9 and 10.
Fig. 9 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one is passing through 24kPa pressure and 600
The contact angle and slide angle of underwater oil when mesh Sandpapering different distance change, and 1 is contact angle, and 2 be slide angle；It can by figure
Know, prepared wear-resisting super hydrophilic underwater super oleophobic coating is in dry state after undergoing abrasion (rub 10cm every time) repeatedly
Its underwater superoleophobic characteristic will not be lost, until coating is completely worn out totally, underwater superoleophobic property is just lost.
Figure 10 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by the embodiment one being spontaneously wet out by water is being passed through
The contact angle and slide angle of underwater oil when 24kPa pressure and 600 mesh Sandpapering different distance change, and 1 is contact angle, and 2 are
Slide angle；As seen from the figure, even if prepared wear-resisting super hydrophilic underwater super oleophobic coating undergoes abrasion repeatedly (every under hygrometric state
Secondary friction 10cm) after will not lose its underwater superoleophobic characteristic, until coating is completely worn out totally, underwater superoleophobic property
Just lose.
Figure 11 is wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one by flow velocity 3.5m/s and straight
The water column of diameter 5mm washes away the photo after 1h, and 1 is water column shock zone；As seen from the figure, prepared super-hydrophilic coating can be fine
Current scour must be resisted.
The intersection of wear-resisting super hydrophilic underwater super oleophobic coating and adhesive layer that Figure 12 is prepared for embodiment one is through overcurrent
The water column of fast 3.5m/s and diameter 5mm wash away the photo after 1h, and 1 is water column shock zone；As seen from the figure, prepared wear-resisting super
There is good bond strength in the junction of hydrophilic underwater super oleophobic coating floating coat and adhesive, fine can must resist water flow punching
Brush.
Figure 13 is that wear-resisting super hydrophilic underwater superoleophobic slide surface prepared by embodiment one is passing through different physics and change
The contact angle and slide angle of underwater oil after learning environmental treatment, " ■ " are contact angle, and " ◆ " is slide angle, and it is -30 that a, which is in temperature,
DEG C air in handle 72h；B is to handle 72h in the air that temperature is 100 DEG C；C is in the deionized water that temperature is 80 DEG C
Processing 12 hours；D is to handle 72h in the aqueous sulfuric acid of pH=1；E is the sodium-chloride water solution that mass percent is 3.5%
Middle processing 72h；F is soak at room temperature 72h in toluene；G is soak at room temperature 72h in ethyl alcohol.As seen from the figure, prepared wear-resisting super parent
Superoleophobic surface has good chemical stability to water under water.
The preparation of the wear-resisting super hydrophilic underwater super oleophobic coating of the present embodiment is by cured adhesive coating progress
Swelling, and realized using the fixed hydrophilic nylon coatings of the process, adhesive used is 92 epoxy resin of Ao Sibang.So
And in practical applications, it is any to be can be used in nylon/formic acid coating by the adhesive or polymer that formic acid is swollen and be consolidated
It is fixed.For example, adhesive for polyurethane is equally applicable in addition to epoxy resin；And organic silicon rubber (PDMS), the materials such as polytetrafluoroethylene (PTFE)
Material can not be used to fix nylon coating due to that can not be swollen by formic acid.
The present embodiment coating containing inorganic particulate is by inorganic SiO2Particle, nylon 6,6 and formic acid (88%) three composition, and
In practical applications, each component can be adjusted on demand: be removed outside nylon 6,6, other nylon series of products such as nylon 6, Buddhist nun
Dragon 4,6 etc. is suitable for the present invention, here without exhaustion；The concentration of formic acid can also be turned up or be reduced according to demand；It removes
SiO2Outside particle, other particles such as TiO2, BaSO4It can also be applied etc. any powder body material that can be used for constructing coating coarse structure
In the present invention, and its particle size range can also be adjusted in wide scope.
Claims (10)
1. a kind of method for preparing wear-resisting super hydrophilic underwater superoleophobic surface based on swelling method, it is characterised in that one kind is based on swelling
The method that method prepares wear-resisting super hydrophilic underwater superoleophobic surface is completed by the following steps:
One, inorganic particulate coating is prepared:
The formic acid that nylon, hydrophilic inorganic particulate and mass percent are 88% is mixed, coating containing inorganic particulate is obtained；
The mass ratio of the nylon and hydrophilic inorganic particulate is 1:(0.5~20)；In the coating containing inorganic particulate
The gross mass percentage of nylon and hydrophilic inorganic particulate is 10%~55%；
Two, glue-line is sprayed:
By adhesive even application in substrate surface, uniform glue-line is obtained, then drying is fully cured to glue-line, obtains gluing
Substrate；
The adhesive is the adhesive that can be swollen by formic acid or can be by the polymer of formic acid swelling；
Three, dip-coating inorganic particulate coating:
By the substrate vertical immersion of gluing in coating containing inorganic particulate, soaking time is 5s~2h, then by the base after immersion
Bottom lifts extraction with the speed of 1mm/s~10mm/s from coating containing inorganic particulate, obtains the substrate for being adsorbed with coating, will adsorb
It is dry in 20 DEG C~80 DEG C baking ovens for having the substrate of coating to be placed in temperature, until solvent volatilizees completely, that is, completes to be based on swelling method
The method for preparing wear-resisting super hydrophilic underwater superoleophobic surface.
2. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that hydrophilic inorganic particulate described in step 1 is SiO2Particle, TiO2Particle or BaSO4Particle.
3. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that nylon described in step 1 is nylon 6,6, nylon 6 or nylon 4,6.
4. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that substrate described in step 2 is acid resisting material.
5. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that adhesive described in step 2 is adhesive for polyurethane or epoxy resin.
6. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
The mass ratio for being characterized in that nylon described in step 1 and hydrophilic inorganic particulate is 1:4.4.
7. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that the gross mass percentage of nylon and hydrophilic inorganic particulate is in coating containing inorganic particulate described in step 1
35%.
8. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that in step 3 by the substrate vertical immersion of gluing in coating containing inorganic particulate, soaking time 10min.
9. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that in step 3 that the substrate after immersion is then lifted extraction with the speed of 2mm/s from coating containing inorganic particulate.
10. a kind of method that wear-resisting super hydrophilic underwater superoleophobic surface is prepared based on swelling method according to claim 1,
It is characterized in that in step 3 that it is drying in 25 DEG C of baking ovens that the substrate for being adsorbed with coating is placed in temperature, until solvent volatilizees completely.
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| CN112159117A (en) * | 2020-10-10 | 2021-01-01 | 东北石油大学 | Method for rapidly preparing underwater super-oleophobic anticorrosive coating |
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| CN102717560A (en) * | 2012-06-13 | 2012-10-10 | 南京工业大学 | Sunlight-initiated organic-inorganic composite self-cleaning coating and preparation method thereof |
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| CN105018910A (en) * | 2015-06-27 | 2015-11-04 | 西安科技大学 | Method for preparing super-oleophobic surface by taking kaolin as raw material |
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| CN102717560A (en) * | 2012-06-13 | 2012-10-10 | 南京工业大学 | Sunlight-initiated organic-inorganic composite self-cleaning coating and preparation method thereof |
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| CN105018910A (en) * | 2015-06-27 | 2015-11-04 | 西安科技大学 | Method for preparing super-oleophobic surface by taking kaolin as raw material |
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