CN102433053A - Coating with gradient contact angle function and preparation method thereof - Google Patents
Coating with gradient contact angle function and preparation method thereof Download PDFInfo
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- CN102433053A CN102433053A CN2011102634370A CN201110263437A CN102433053A CN 102433053 A CN102433053 A CN 102433053A CN 2011102634370 A CN2011102634370 A CN 2011102634370A CN 201110263437 A CN201110263437 A CN 201110263437A CN 102433053 A CN102433053 A CN 102433053A
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- 239000011248 coating agent Substances 0.000 title claims abstract description 84
- 238000000576 coating method Methods 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000000178 monomer Substances 0.000 claims abstract description 52
- 239000000243 solution Substances 0.000 claims abstract description 51
- 229920000642 polymer Polymers 0.000 claims abstract description 26
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract 6
- 238000006116 polymerization reaction Methods 0.000 claims description 42
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229920003180 amino resin Polymers 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 4
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- 239000005711 Benzoic acid Substances 0.000 claims description 3
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 3
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 235000010233 benzoic acid Nutrition 0.000 claims description 3
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 claims description 3
- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 claims description 2
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 2
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical group COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- ATZHWSYYKQKSSY-UHFFFAOYSA-N tetradecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCOC(=O)C(C)=C ATZHWSYYKQKSSY-UHFFFAOYSA-N 0.000 claims description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims 4
- LGJCFVYMIJLQJO-UHFFFAOYSA-N 1-dodecylperoxydodecane Chemical compound CCCCCCCCCCCCOOCCCCCCCCCCCC LGJCFVYMIJLQJO-UHFFFAOYSA-N 0.000 claims 2
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 claims 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims 2
- 235000019400 benzoyl peroxide Nutrition 0.000 claims 2
- 238000002156 mixing Methods 0.000 claims 2
- 150000002978 peroxides Chemical class 0.000 claims 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims 1
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims 1
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims 1
- CYUZOYPRAQASLN-UHFFFAOYSA-N 3-prop-2-enoyloxypropanoic acid Chemical compound OC(=O)CCOC(=O)C=C CYUZOYPRAQASLN-UHFFFAOYSA-N 0.000 claims 1
- GGBJHURWWWLEQH-UHFFFAOYSA-N Butyl-cyclohexane Natural products CCCCC1CCCCC1 GGBJHURWWWLEQH-UHFFFAOYSA-N 0.000 claims 1
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical group CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 claims 1
- 239000012153 distilled water Substances 0.000 claims 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims 1
- 239000012948 isocyanate Substances 0.000 claims 1
- 150000002513 isocyanates Chemical class 0.000 claims 1
- HMZGPNHSPWNGEP-UHFFFAOYSA-N octadecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C(C)=C HMZGPNHSPWNGEP-UHFFFAOYSA-N 0.000 claims 1
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 claims 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 claims 1
- 239000008096 xylene Substances 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 description 27
- 238000004140 cleaning Methods 0.000 description 19
- 238000009835 boiling Methods 0.000 description 18
- 238000010438 heat treatment Methods 0.000 description 10
- -1 YLENE Chemical compound 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- ZQMIGQNCOMNODD-UHFFFAOYSA-N diacetyl peroxide Chemical compound CC(=O)OOC(C)=O ZQMIGQNCOMNODD-UHFFFAOYSA-N 0.000 description 6
- 150000002148 esters Chemical class 0.000 description 5
- 229920001684 low density polyethylene Polymers 0.000 description 4
- 239000004702 low-density polyethylene Substances 0.000 description 4
- 230000003075 superhydrophobic effect Effects 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 125000004494 ethyl ester group Chemical group 0.000 description 3
- DSCFFEYYQKSRSV-UHFFFAOYSA-N 1L-O1-methyl-muco-inositol Natural products COC1C(O)C(O)C(O)C(O)C1O DSCFFEYYQKSRSV-UHFFFAOYSA-N 0.000 description 2
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- VVWRJUBEIPHGQF-UHFFFAOYSA-N propan-2-yl n-propan-2-yloxycarbonyliminocarbamate Chemical compound CC(C)OC(=O)N=NC(=O)OC(C)C VVWRJUBEIPHGQF-UHFFFAOYSA-N 0.000 description 2
- AYEFIAVHMUFQPZ-UHFFFAOYSA-N propane-1,2-diol;prop-2-enoic acid Chemical class CC(O)CO.OC(=O)C=C AYEFIAVHMUFQPZ-UHFFFAOYSA-N 0.000 description 2
- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical class CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000001117 sulphuric acid Substances 0.000 description 2
- 235000011149 sulphuric acid Nutrition 0.000 description 2
- ZMARGGQEAJXRFP-UHFFFAOYSA-N 1-hydroxypropan-2-yl 2-methylprop-2-enoate Chemical compound OCC(C)OC(=O)C(C)=C ZMARGGQEAJXRFP-UHFFFAOYSA-N 0.000 description 1
- GWZMWHWAWHPNHN-UHFFFAOYSA-N 2-hydroxypropyl prop-2-enoate Chemical compound CC(O)COC(=O)C=C GWZMWHWAWHPNHN-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical group CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229940043232 butyl acetate Drugs 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Landscapes
- Polymerisation Methods In General (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Paints Or Removers (AREA)
Abstract
本发明公开一种具有梯度接触角功能涂层及其制备方法。首先将单体和引发剂在密闭容器内混合，得到第一、第二预聚单体，分别加到含有溶剂的容器中，加热搅拌3～6小时，得到聚合物溶液；再将聚合物溶液与固化剂混合，涂覆于底材上，在110～170℃下加热固化10～40分钟；最后将固化涂层置于敞口容器中，向容器中缓慢滴加水溶液，在3～8小时滴加完毕时，底材上沿刚好被水溶液完全浸润，并将得到的预功能涂层清洗2～3次，40～60℃下干燥，制得具有梯度接触角功能涂层。接触角能在95°±5°～15°±5°范围内呈连续梯度变化，并可在不同底材上实现，制备方法简单易行，成本低廉，扩展了梯度接触角功能涂层的应用范围。The present invention discloses a functional coating with a gradient contact angle and a preparation method thereof. First, a monomer and an initiator are mixed in a closed container to obtain a first and a second prepolymer monomer, which are added to a container containing a solvent, heated and stirred for 3 to 6 hours to obtain a polymer solution; then the polymer solution is mixed with a curing agent, coated on a substrate, and heated and cured at 110 to 170°C for 10 to 40 minutes; finally, the cured coating is placed in an open container, and an aqueous solution is slowly dripped into the container. When the dripping is completed in 3 to 8 hours, the upper edge of the substrate is just completely infiltrated by the aqueous solution, and the obtained pre-functional coating is washed 2 to 3 times, and dried at 40 to 60°C to obtain a functional coating with a gradient contact angle. The contact angle can change continuously in a gradient within the range of 95°±5° to 15°±5°, and can be realized on different substrates. The preparation method is simple and easy, low in cost, and expands the application range of the gradient contact angle functional coating.
Description
Technical field
The present invention relates to field of functional materials, particularly a kind of functional coating and preparation technology thereof with contact angle continuity variation characteristic.
Background technology
FGM is meant the function of material, changes continuously with space or time or a kind of high performance material of stepped change like component, structure, performance.Contact angle is the important physical amount that is used for weighing the material surface wettability, and general contact angle is more little, and surface energy is big more.Gradient contact angle surface refers to that certain direction gradient continuity changes the material surface contact angle along the surface.Because the peculiar property on gradient contact angle surface, it moves at drop, microfluidic flow, and fields such as biological absorption and efficient heat transfer have shown broad prospect of application.
The existing preparation in the method for gradient contact angle material, ground there is high requirement.Such as; " the Surface Gradient Material:From Superhydrophobicity to Superhydrophilicity " that X.Zhang etc. deliver in " Langmuir " (2006 the 22nd volume the 4483rd～4486 page) (gradient surface material: from super-hydrophobic to the ultra hydrophilic) article; Through the self-assembly effect, realized the transformation of surface contact angle from super-hydrophobic (156.4 °) to ultra hydrophilic (＜10 °) at coarse gold at the end; At first obtain having the coarse gold end of micro-nano dual microtexture through electrodip process; Then, through changing the drips of solution acceleration stresses, on ground, formed contact angle continually varying gradient surface, rate of addition is slow more, and the gradient contact angle variation range that obtains is big more.In addition; Y.C.Han etc. are in " Low-Density Polyethylene (LDPE) Surface With a Wettability Gradient by Tuning its Microstructures " (regulation and control new LDPE (film grade) surface microscopic topographic makes up the gradient wetted surface) article that " Macromolecular Rapid Communications " (volume was the 637th～642 page in 2005 the 26th) delivered; (the contact angle: 165.8 ° of pointing out to have porous super hydrophobic; Roll angle: 4 °) new LDPE (film grade) (LPDE) on surface places in the gradient temperature field, and the temperature in hot junction is higher than the melting temperature T m of LPDE, in the temperature field, places after 10 minutes; Because the surperficial crystalline structure in hot junction is destroyed; The surface high porosity reduces, and hydrophobicity descends, so in the direction that raises along temperature; Surface microstructure forms graded, has formed the gradient wetted surface from super-hydrophobic to hydrophobic with this.More than prepare in the method on gradient contact angle surface, ground is required height, the ground that requires that has has the self-assembly characteristic, and the ground that requires that has has certain susceptibility to temperature; These preparing methods have limited the further application on gradient contact angle surface.
Summary of the invention
The object of the present invention is to provide a kind of simply, effectively, have coating of gradient contact angle characteristic and preparation method thereof.The preparation method of this functional coating can not only successfully prepare the functional coating of contact angle graded, can also on multiple unlike material ground, realize the graded of contact angle.
The object of the invention is realized through following technical scheme: a kind of preparation method with gradient contact angle functional coating is characterized in that comprising the steps:
The first step in mass fraction, with after 100～400 part of first monomer mixes, stirs 5～20 part of first initiator 10～20 minutes with 30～80 rev/mins rotating speeds, obtains the first pre-polymerization monomer;
In second step,, 5～20 part of second initiator with after 500～1000 part of second monomer mixes, with 30～80 rev/mins rotating speeds stirrings 10～30 minutes, obtained the second pre-polymerization monomer in mass fraction;
In the 3rd step, in mass fraction, the first pre-polymerization monomer dropping that the first step is obtained is to filling 900～3500 parts of solvents; Stir speed (S.S.) is in 250～400 rev/mins the container; In 0～60 minute, dropwise, the second pre-polymerization monomer that again second step was obtained progressively is added drop-wise in the said vesse, in 20～60 minutes, dropwises; At last, obtain polymers soln with 90～140 ℃ temperature heated and stirred 3～6 hours;
In the 4th step,, the 3rd polymers soln that obtain of step with after 1～5 part of solidifying agent mixes, with 50～80 rev/mins rotating speeds stirrings 10～30 minutes, is obtained Procuring solution in mass fraction;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the ground of surface cleaning, is warmed up to 110～170 ℃, and thermostatically heating was solidified 10～40 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the aqueous solution gradually, guarantees when dropwising in 3～8 hours, and the ground upper edge is just soaked into fully, obtains preparatory functional coating;
The 7th step, after the 6th step, the preparatory functional coating that obtains placed zero(ppm) water to clean 2～3 times, 40～60 ℃ dry down, after the drying, obtain having gradient contact angle functional coating.
First initiator described in the step 1 is a kind of in Diisopropyl azodicarboxylate, Lucidol, acetylperoxide, peroxo-12 phosphinylidynes, the dicumyl peroxide; Said first monomer is a kind of in Rocryl 400, Rocryl 410, vinylformic acid carboxylic ethyl ester, the Propylene glycol monoacrylate.
Said second initiator of step 2 is a kind of in Diisopropyl azodicarboxylate, Lucidol, acetylperoxide, peroxo-12 phosphinylidynes, the dicumyl peroxide; Said second monomer is more than one in TEB 3K, Jia Jibingxisuanyizhi, propyl methacrylate, n-BMA, Propenoic acid, 2-methyl, isobutyl ester, methacrylic tert-butyl acrylate, methylacrylic acid tetradecyl ester, methylacrylic acid stearyl, methyl acrylate, ethyl propenoate, n-butyl acrylate, NSC 20949 and the tert-butyl acrylate.
The said solvent of step 3 is more than one in toluene, YLENE, butylacetate and the hexanaphthene.
The said solidifying agent of step 4 is aminoresin or isocyanic ester.
The said ground of step 5 is aluminium, copper, silver, gold, silicon or slide glass.
The said aqueous solution of step 6 is that concentration is sodium hydroxide solution, potassium hydroxide solution, hydrochloric acid soln, sulphuric acid soln, phosphoric acid solution, benzoic acid solution, sodium carbonate solution, phospho-wolframic acid and the salts solution thereof of 0.01mol/L～10mol/L, in the sodium dodecyl sulfate solution more than one.
Described gradient contact angle continuity monotone variation.
Said gradient contact angle variation range is 95 ° ± 5 °～15 ° ± 5 °.
A kind of have a gradient contact angle functional coating, by method for preparing.
Gradient contact angle coating provided by the present invention belongs to field of functional materials.
The present invention is combined into the basis with radical polymerization; Prepare the methyl acrylic ester resin solution through solvent polymerization method; And carry out crosslinked with solidifying agent; On ground, form the densified polymer film,, form gradient contact angle surface with certain wetting scope through changing the solution immersion time and soaking into concentration.The present invention has not only successfully prepared the gradient wetted surface, and because the coating characteristic of synthetic resins, has enlarged the range of choice of ground, for solid foundation has been laid in the further application of gradient wetted surface.
The present invention compared with prior art has following advantage and beneficial effect:
(1) prepared functional coating has the characteristic of the continuous monotone variation of gradient contact angle.
(2) prepared functional coating can be realized contact angle variation within the specific limits.
(3) prepared functional coating can be realized on grounds such as aluminium, copper, silver, gold, silicon or slide glass, has enlarged the range of choice of ground, for solid foundation has been laid in the further application of gradient wetted surface.
(4) prepared functional coating has good film performance.
(5) raw material of the present invention obtains easily, and the preparation method is simple, and is with low cost, helps further popularization.
Embodiment
Below in conjunction with embodiment the present invention is done further detailed explanation, but embodiment of the present invention is not limited thereto.
Embodiment 1
The first step, 15 gram Diisopropyl azodicarboxylates and 260 are restrained Rocryl 400s, and to join rotating speed be in 60 rev/mins the airtight magnetic stirring apparatus, stirred 15 minutes, obtains the first pre-polymerization monomer;
In second step, in mass fraction, 15 gram Diisopropyl azodicarboxylates and 800 are restrained TEB 3Ks, and to join rotating speed be in 60 rev/mins the airtight magnetic stirring apparatus, stirred 20 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 2300 gram toluene, and stir speed (S.S.) is in 330 rev/mins the four-hole boiling flask, in 45 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 40 minutes, dropwise, 110 ℃ of heated and stirred 5 hours obtain polymers soln;
The 4th step restrained aminoresin with the 3rd polymers soln that obtains of step and 3 and mixes, and joined rotating speed and was in 60 rev/mins the airtight magnetic stirring apparatus, stirred 20 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the aluminium flake of surface cleaning, and the baking oven of putting into 120 ℃ was heating and curing 30 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the sodium hydroxide solution that concentration is 0.02mol/L gradually, and after 3 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 3 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 40 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 100 ° of infiltrating time from long 20 ° of infiltrating time.
Embodiment 2
The first step, 10 gram dicumyl peroxides and 320 are restrained Propylene glycol monoacrylates, and to join rotating speed be in 40 rev/mins the airtight magnetic stirring apparatus, stirred 10 minutes, obtains the first pre-polymerization monomer;
In second step, 8 gram Lucidols and 900 are restrained the methacrylic tert-butyl acrylates, and to join rotating speed be in 45 rev/mins the airtight magnetic stirring apparatus, stirred 28 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained is added to and fills 3200 gram butylacetates; Stir speed (S.S.) is in 330 rev/mins the four-hole boiling flask, and the second pre-polymerization monomer dropping that again second step was obtained dropwised in 30 minutes in four-hole boiling flask; 120 ℃ of heated and stirred 3 hours obtain polymers soln;
The 4th step restrained aminoresin with the 3rd polymers soln that obtains of step and 1.5 and mixes, and joined rotating speed and was in 80 rev/mins the airtight magnetic stirring apparatus, stirred 18 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the silver strip of surface cleaning, and the baking oven of putting into 115 ℃ was heating and curing 38 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the sodium carbonate solution that concentration is 0.07mol/L gradually, and after 7.5 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 2 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 55 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 92 ° of infiltrating time from long 17 ° of infiltrating time.
Embodiment 3
The first step, 8 gram Lucidols and 175 are restrained Rocryl 410s, and to join rotating speed be in 55 rev/mins the airtight magnetic stirring apparatus, stirred 13 minutes, obtains the first pre-polymerization monomer;
In second step, 14.5 gram Lucidols and 920 are restrained methyl acrylates, and to join rotating speed be in 55 rev/mins the airtight magnetic stirring apparatus, stirred 17 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 2250 gram hexanaphthenes, and stir speed (S.S.) is in 270 rev/mins the four-hole boiling flask, in 38 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 27 minutes, dropwise, 125 ℃ of heated and stirred 4.8 hours obtain polymers soln;
The 4th step restrained isocyanic ester with the 3rd polymers soln that obtains of step and 3.7 and mixes, and joined rotating speed and was in 65 rev/mins the airtight magnetic stirring apparatus, stirred 18 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the copper sheet of surface cleaning, and the baking oven of putting into 120 ℃ was heating and curing 12 minutes, obtained solidified coating;
The 6th step; The 5th solidified coating that obtain of step is vertically placed in the open container, and in container, to drip concentration gradually be the hydrochloric acid soln of 5mol/L and the Salkowski's solution of 0.0001mol/L, after 3.2 hours dropping time; The ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 3 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 47 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 100 ° of infiltrating time from long 12 ° of infiltrating time.
Embodiment 4
The first step, 20 gram Lucidols and 380 are restrained Rocryl 410s, and to join rotating speed be in 80 rev/mins the airtight magnetic stirring apparatus, stirred 20 minutes, obtains the first pre-polymerization monomer;
In second step, 20 gram Diisopropyl azodicarboxylates and 300 gram TEB 3Ks and 700 are restrained NSC 20949s, and to join rotating speed be in 80 rev/mins the airtight magnetic stirring apparatus, stirred 30 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 3500 gram YLENE, and stir speed (S.S.) is in 400 rev/mins the four-hole boiling flask, in 58 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 60 minutes, dropwise, 130 ℃ of heated and stirred 6 hours obtain polymers soln;
The 4th step restrained isocyanic ester with the 3rd polymers soln that obtains of step and 5 and mixes, and joined rotating speed and was in 75 rev/mins the airtight magnetic stirring apparatus, stirred 30 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the copper sheet of surface cleaning, and the baking oven of putting into 110 ℃ was heating and curing 40 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the sulphuric acid soln that concentration is 1mol/L gradually, and after 6 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 3 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 50 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 90 ° of infiltrating time from long 10 ° of infiltrating time.
Embodiment 5
The first step, 19 gram peroxo-12 phosphinylidynes and 395 are restrained vinylformic acid carboxylic ethyl esters, and to join rotating speed be in 77 rev/mins the airtight magnetic stirring apparatus, stirred 12 minutes, obtains the first pre-polymerization monomer;
In second step, 17 gram acetylperoxides and 100 gram n-BMAs and 570 are restrained n-butyl acrylates, and to join rotating speed be in 77 rev/mins the airtight magnetic stirring apparatus, stirred 26 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 3450 gram YLENE, and stir speed (S.S.) is in 370 rev/mins the four-hole boiling flask, in 25 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 58 minutes, dropwise, 135 ℃ of heated and stirred 3.4 hours obtain polymers soln;
The 4th step restrained aminoresin with the 3rd polymers soln that obtains of step and 3.6 and mixes, and joined rotating speed and was in 78 rev/mins the airtight magnetic stirring apparatus, stirred 29 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the aluminium flake of surface cleaning, and the baking oven of putting into 113 ℃ was heating and curing 18 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the sodium carbonate solution that concentration is 7mol/L gradually, and after 5.5 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 3 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 50 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 90 ° of infiltrating time from long 20 ° of infiltrating time.
Embodiment 6
The first step, 12 gram acetylperoxides and 350 are restrained vinylformic acid carboxylic ethyl esters, and to join rotating speed be in 50 rev/mins the airtight magnetic stirring apparatus, stirred 18 minutes, obtains the first pre-polymerization monomer;
In second step, 10 gram dicumyl peroxides and 750 are restrained Propenoic acid, 2-methyl, isobutyl esters, and to join rotating speed be in 70 rev/mins the airtight magnetic stirring apparatus, stirred 25 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 500 gram toluene and 2200 gram butylacetates, and stir speed (S.S.) is in 380 rev/mins the four-hole boiling flask, in 40 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 50 minutes, dropwise, 115 ℃ of heated and stirred 4.5 hours obtain polymers soln;
The 4th step restrained isocyanic ester with the 3rd polymers soln that obtains of step and 4.5 and mixes, and joined rotating speed and was in 68 rev/mins the airtight magnetic stirring apparatus, stirred 28 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the silicon chip of surface cleaning, and the baking oven of putting into 140 ℃ was heating and curing 28 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the phosphoric acid solution that concentration is 5mol/L gradually, and after 4.8 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 2 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 45 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 98 ° of infiltrating time from long 13 ° of infiltrating time.
Embodiment 7
The first step, 9 gram Diisopropyl azodicarboxylates and 240 are restrained Rocryl 400s, and to join rotating speed be in 69 rev/mins the airtight magnetic stirring apparatus, stirred 14 minutes, obtains the first pre-polymerization monomer;
In second step, 6 gram dicumyl peroxides and 540 are restrained the methacrylic tert-butyl acrylates, and to join rotating speed be in 78 rev/mins the airtight magnetic stirring apparatus, stirred 24 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 1000 gram toluene and 1000 gram YLENE, and stir speed (S.S.) is in 380 rev/mins the four-hole boiling flask, in 55 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 32 minutes, dropwise, 135 ℃ of heated and stirred 5.5 hours obtain polymers soln;
The 4th step restrained aminoresin with the 3rd polymers soln that obtains of step and 2.2 and mixes, and joined rotating speed and was in 75 rev/mins the airtight magnetic stirring apparatus, stirred 18 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the slide glass of surface cleaning, and the baking oven of putting into 165 ℃ was heating and curing 35 minutes, obtained solidified coating;
The 6th step; The solidified coating that the 5th step was obtained is vertically placed in the open container; And in container, drip potassium hydroxide solution that concentration is 9mol/L and the phospho-wolframic acid one substituted ammonium salt solution of 0.0005mol/L gradually; After 7.7 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 2 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 58 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 99 ° of infiltrating time from long 13 ° of infiltrating time.
Embodiment 8
The first step, 7 gram peroxo-12 phosphinylidynes and 180 are restrained Propylene glycol monoacrylates, and to join rotating speed be in 67 rev/mins the airtight magnetic stirring apparatus, stirred 13 minutes, obtains the first pre-polymerization monomer;
In second step, 14 gram dicumyl peroxides and 200 gram ethyl propenoates and 550 are restrained the methylacrylic acid stearyl, and to join rotating speed be in 67 rev/mins the airtight magnetic stirring apparatus, stirred 18 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 450 gram YLENE and 2100 gram toluene, and stir speed (S.S.) is in 320 rev/mins the four-hole boiling flask, in 48 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 55 minutes, dropwise, 135 ℃ of heated and stirred 4.8 hours obtain polymers soln;
The 4th step restrained aminoresin with the 3rd polymers soln that obtains of step and 3.6 and mixes, and joined rotating speed and was in 78 rev/mins the airtight magnetic stirring apparatus, stirred 24 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the slide glass of surface cleaning, and the baking oven of putting into 160 ℃ was heating and curing 35 minutes, obtained solidified coating;
In the 6th step, the solidified coating that the 5th step was obtained is vertically placed in the open container, and in container, drips the benzoic acid solution that concentration is 0.75mol/L gradually, and after 8 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 2 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 55 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 100 ° of infiltrating time from long 20 ° of infiltrating time.
Embodiment 9
The first step, 17 gram Lucidols and 190 are restrained Rocryl 400s, and to join rotating speed be in 75 rev/mins the airtight magnetic stirring apparatus, stirred 18 minutes, obtains the first pre-polymerization monomer;
In second step, in mass fraction, 19 gram Diisopropyl azodicarboxylates and 200 gram TEB 3Ks and 700 are restrained n-butyl acrylates, and to join rotating speed be in 78 rev/mins the airtight magnetic stirring apparatus, stirred 27 minutes, obtains the second pre-polymerization monomer;
The 3rd step; The first pre-polymerization monomer that the first step is obtained progressively is added drop-wise to and fills 1500 gram YLENE and 1700 gram hexanaphthenes, and stir speed (S.S.) is in 385 rev/mins the four-hole boiling flask, in 58 minutes, to dropwise; Again with the second second pre-polymerization monomer dropping that obtain of step in four-hole boiling flask; In 55 minutes, dropwise, 138 ℃ of heated and stirred 3.5 hours obtain polymers soln;
The 4th step in mass fraction, restrained isocyanic ester with the 3rd polymers soln that obtains of step and 1.3 and mixes, and joined rotating speed and was in 78 rev/mins the airtight magnetic stirring apparatus, stirred 26 minutes, obtained Procuring solution;
In the 5th step, the Procuring solution that the 4th step was obtained evenly is coated on the copper sheet of surface cleaning, and the baking oven of putting into 116 ℃ was heating and curing 14 minutes, obtained solidified coating;
The 6th step; The solidified coating that the 5th step was obtained is vertically placed in the open container; And in container, to drip concentration gradually be the sodium hydroxide solution of 1mol/L and the sodium dodecyl sulfate solution of 0.0002mol/L; After 7.8 hours dropping time, the ground upper edge is soaked into fully, obtains preparatory functional coating;
The 7th step placed zero(ppm) water to clean 3 times the 6th preparatory functional coating that obtain of step, and after the cleaning, 46 ℃ dry down, after the drying, accomplishes the preparation with gradient contact angle functional coating, and contact angle increases to short 96 ° of infiltrating time from long 11 ° of infiltrating time.
Claims (10)
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| CN110434337A (en) * | 2019-08-23 | 2019-11-12 | 广州番禺职业技术学院 | A kind of 3D printing prepares the preparation method of bionic intelligence metal material surface |
| CN115156004A (en) * | 2022-08-08 | 2022-10-11 | 广州番禺职业技术学院 | A kind of preparation method of patterned gradient wetting functional surface with biocompatibility |
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| US5098972A (en) * | 1989-04-28 | 1992-03-24 | Atochem | Hardenable, fluorinated copolymer, process for its manufacture and its application in varnishes and paints |
| CN101914185A (en) * | 2010-09-08 | 2010-12-15 | 廊坊金汇利工业涂料有限公司 | Hydroxy acrylic resin aqueous dispersion and water-based coating prepared therefrom |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5098972A (en) * | 1989-04-28 | 1992-03-24 | Atochem | Hardenable, fluorinated copolymer, process for its manufacture and its application in varnishes and paints |
| CN101914185A (en) * | 2010-09-08 | 2010-12-15 | 廊坊金汇利工业涂料有限公司 | Hydroxy acrylic resin aqueous dispersion and water-based coating prepared therefrom |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110434337A (en) * | 2019-08-23 | 2019-11-12 | 广州番禺职业技术学院 | A kind of 3D printing prepares the preparation method of bionic intelligence metal material surface |
| CN115156004A (en) * | 2022-08-08 | 2022-10-11 | 广州番禺职业技术学院 | A kind of preparation method of patterned gradient wetting functional surface with biocompatibility |
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