CN102675941A - Ultraviolet (UV) curable super-hydrophobic anti-fingerprint coating and preparation method thereof - Google Patents
Ultraviolet (UV) curable super-hydrophobic anti-fingerprint coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an ultraviolet (UV) curable super-hydrophobic anti-fingerprint coating, which consists of a polyurethane acrylate (PUA) resin, an acrylic ester resin, an activated fluorine monomer, a silicon resin and modified nano SiO2. The UV curable coating consists of a PUA oligomer, an activated thinner, a photoinitiator and an additive. According to the UV curable super-hydrophobic anti-fingerprint coating, the UV curable coating is prepared from the high-activity PUA oligomer, the activated thinner, the photoinitiator and the like, and a monomer with a special structure is added to resist fingerprint impressions; on such a basis, the activated fluorine monomer, the silicon resin and the like are introduced to form surface-dense and stable self-demixing hydrophobic varnish, so that a self-cleaning effect is achieved; and the modified nano SiO2 is used for constructing a surface micro/nanostructure by adopting a self-assembly technology, so that the UV curable super-hydrophobic anti-fingerprint coating has high performance. The invention also discloses a preparation method for the UV curable super-hydrophobic anti-fingerprint coating.
Description
Technical field
The present invention relates to a kind of UV solidified coating, relate in particular to a kind of UV and solidify super-hydrophobic fingerprint-resistant coating and preparation method thereof.
Background technology
UV solidifies super-hydrophobic fingerprint-resistant coating with its technology, economy and ecological dominance, and really must deserve to be called " 5E " type environmental protection coating material.Estimate that range of application can be extremely wide, rate of growth can be exceedingly fast, and will be penetrated into the speciality coating industry gradually.Some kind (like epoxy, chlorinated rubber etc.) defencive function is good and decorate properties is poor slightly in the traditional coating, and some kind (like pyroxylin(e)finish) is good decorative property and defencive function is poor then.Yet polyurethane coating has protection and decorate properties concurrently, and has high degree of mechanical wear resistance and toughness, has wide range of applications.
Radiation curing technology is with " 5E " characteristics that it was had; I.e. efficient (Efficient); Wide adaptability (Enabling); Economical (Economical), energy-conservation (Energy Saving) and environmental friendliness (Environmental) have become the very swift and violent a kind of novel green technology of development since coming out the sixties in 20th century.China has developed at present after the U.S., Japan, the global the third-largest radiation curing product place of production, and this is wherein maximum with photo-cured coating output again.Though the photo-cured coating output of China has occupied prostatitis, the world, in general, product technology content is lower, and added value is not high, the main dependence on import of many resin materials and additive.In the process of the new high-tech industry that radiation curing led, the radiation curing product substitutes traditional product gradually with its " 5E ", and large quantities of correlation technique industries have been grown in its application and extensive.UV-light (UV) curing technology belongs to a kind of of radiation curing, accounts for global radiation at present and solidifies 90% more than of industry, and wherein, the coating material solidified industry of UV accounts for about 2/3.Coating material solidified bamboo-wood floor coating, plastic paint, paper glazing paint, metallic paint, vacuum metallizing coating, powder coating, antistatic/conductive coating, the release coating etc. of mainly containing of UV.To the present both at home and abroad coating material solidified current situation of UV, UV is coating material solidified to become development trend from now on to the speciality coating development.
Summary of the invention
To above-mentioned technological deficiency; Technical problem to be solved by this invention provides characteristics such as coating material solidified efficient, the wide adaptability that has of a kind of UV of having, economy, energy-conservation and environmental friendliness, and the UV that has surperficial automatically cleaning effect, surface anticorrosion, hydrophobicity characteristics simultaneously solidifies super-hydrophobic fingerprint-resistant coating and preparation method thereof.
In order to solve the problems of the technologies described above, the present invention takes following technical scheme: a kind of UV solidifies super-hydrophobic fingerprint-resistant coating, and this coating is by polyurethane acrylate resin, acrylate resin, active fluorine monomer, silicone resin and modified Nano SiO
2Form; Described UV cured coating film is made up of urethane acrylate oligomer, reactive thinner, light trigger and auxiliary agent.This coating each component concentration by mass percentage is: polyurethane acrylate resin 25-50.45%, acrylate resin 10-15%, active fluorine monomer 0.5-5%, silicone resin 5-10%; Modified manometer silicon dioxide 1-4%; Reactive thinner 5-7%, light trigger 0.05-1%, auxiliary agent 28-33%.UV solidify super-hydrophobic fingerprint-resistant coating adopt highly active PUA oligopolymer, reactive thinner, and light trigger etc. to process UV coating material solidified, add the monomer opposing fingerprint trace of special construction; On this basis, introduce active fluorine monomer, silicone resin etc. and form surface compacts, stable, thereby reach the automatically cleaning effect from the hydrophobic varnish of layering; And through modified Nano SiO
2Adopt self-assembling technique to make up the UV that surface micronano structure makes it to become excellent performance and solidify super-hydrophobic fingerprint-resistant coating.
Further, described urethane acrylate oligomer is generated by hexamethylene diisocyanate trimer and Propylene glycol monoacrylate reaction, and this urethane acrylate oligomer is a small molecular weight three-functionality-degree urethane acrylate oligomer.Because the photopolymerization reaction of oligopolymer urethane acrylate (PUA) is active in epoxy acrylate; Curing speed is slow, viscosity is high; Greatly limited it and done the application of oligopolymer, the excellent properties of urethane can not well be used in UV is coating material solidified.So; Urethane acrylate oligomer of the present invention selects for use the reaction of hexamethylene diisocyanate trimer (HDI tripolymer) and Propylene glycol monoacrylate (HPA) to generate small molecular weight three-functionality-degree urethane acrylate (PUA) oligopolymer, each molecule contains six polarity carbamate groups and three active unsaturated double-bonds, when having increased coating to the sticking power of base material; Greatly increased laser curing velocity; Overcome the drawback of conventional P UA oligopolymer, kept the excellent properties that urethane itself is had, enlarged PUA solidifies oligopolymer as UV range of application; Adopt the monomer of special construction to participate in polymerization, make the very anti-fingerprint of coatingsurface.
Further, described acrylate resin is synthesized by TEB 3K, methyl acrylate, Bing Xisuandingzhi, and this acrylate resin is a LV high-solid content acrylic acid ester resin.Select TEB 3K (MMA), methyl acrylate (MA), Bing Xisuandingzhi synthetic LV high-solid content acrylic acid ester resins such as (BA) for use; Institute's synthetic resin has low surface energy; Except performances such as the sticking power of UV cured coating film, weathering resistance, chemical resistance are improved; Regulate the second-order transition temperature (Tg) and the film forming properties of coating; Form self stratifying coating with UV curing system cured process in addition, the low surface energy polyacrylate resin is that coating surface forms low surface energy structures.
Further, described acrylate resin is synthesized by TEB 3K, Bing Xisuandingzhi, vinylbenzene, vinyl cyanide.The polyacrylate resin of preparation LV high solids content; Select low surface energy acrylate monomer (TEB 3K, Bing Xisuandingzhi, vinylbenzene, vinyl cyanide etc.) for use; Through factors such as control initiator amount, chain-transfer agent consumption, polymerization temperature, polymerization times, prepare the polyacrylate resin of LV high solids content with low surface energy.In the UV curing system, the varnish transmittance is not being produced under the prerequisite of considerable influence; Utilize the low surface property of polymethacrylate resin to be easier to solidification process generation layered structure; Thereby form the low surface energy hydrophobic structure, utilize the monomer of special construction can resist fingerprint trace significantly.On the other hand, to have given UV equally coating material solidified to the good sticking power of base material, coating transmittance and other mechanical property for the polymethacrylate resin of small molecular weight.
Further, described light trigger is by 1-hydroxy cyclohexyl phenylketone and 2,4, and these two kinds of light triggers of 6-trimethylbenzoyl diphenyl phosphine oxide are formed.Light trigger can produce radical as photodestruciton type composite initiation system in the broad ultraviolet region, accomplish the fast setting of system; Select the reactive thinner of different functionality for use, in the photocuring process, cooperate PUA oligopolymer generation crosslinking reaction, when playing diluting effect, regulate the second-order transition temperature and the performance of solidifying back coating.
Further, described active fluorine monomer is high reactivity, fluorine content height and has lower surfactivity and have low surface-active fluorine monomer.The fluorine monomer of employing low surface energy and silicone resin etc.; The UV curing system is in solvent evaporates, drying and solidification process; Be separated with common generation of acrylate resin, surfactivity can be automatically migrated to film coated surface by low material, wherein silicone resin film forming automatically; Active fluorine monomer migrate to the surface and in the UV solidification process with system oligopolymer, reactive thinner take place crosslinked, thereby form fine and close, stable low surface energy hydrophobic structure.
In addition, the invention still further relates to the preparation method that a kind of UV solidifies super-hydrophobic fingerprint-resistant coating, this preparing method's step is:
(1) adopt hexamethylene diisocyanate trimer and Propylene glycol monoacrylate under catalyzer and stopper effect, to carry out single step reaction, generation has the three-functionality-degree urethane acrylate oligomer of high reaction activity small molecular weight, solidifies oligopolymer as UV; The reactive thinner that adds different functionality, the performance of regulating the active of photocuring reaction and solidifying the back paint film; Add 1-hydroxy cyclohexyl phenylketone and 2,4,6-trimethylbenzoyl diphenyl phosphine oxide is as light trigger; Introduce acrylate resin and improve curing performance, and regulate the second-order transition temperature and the film-forming properties of paint film;
(2) adopt high reactivity, fluorine content is high and the silicone resin that has lower surfactivity and have low surface-active fluorine monomer, a high heat resistance as the low surface energy material; In solvent evaporates, drying and solidification process; Be automatically migrated to coatingsurface, it is crosslinked through UV curing coatingsurface fluorine monomer and the inner oligopolymer of system, reactive thinner to be taken place, in addition; Acrylate resin, silicone resin be film forming automatically, thereby makes coatingsurface form densification, stable low surface energy hydrophobic structure;
(3) employing is carried out chemically modified and parcel to nanoparticle surface, forms dewatering nano SiO
2, through the nanometer SiO after the modification
2The surface is than strong-hydrophobicity and has the functional functional group that can react, adds in the UV curing system, makes up the surperficial micro nano structure of varnish with secondary composite structure and the surface hydrophobicity that it was had, and makes UV and solidifies super-hydrophobic fingerprint-resistant coating.
The present invention compared with prior art, its advantage is:
(1) overcome that conventional urethane propenoate activity is low, curing speed is slow, viscosity greatly, the defective seldom used as oligopolymer; It is little to invent prepared urethane acrylate oligomer molecular weight, and viscosity is low; Contain six strong polarity carbamate groups and three high reactivity unsaturated double-bonds in each molecule, in the performance of having improved coating and sticking power, accelerated laser curing velocity, satisfy the requirement of modern industry development base material;
(2) adopt silicone resin and high reactivity fluorine monomer as the low surface energy material; Because the performances such as excellent optics, thermotolerance, surperficial water repellency and spontaneous film forming that silicone resin had; Make its reach the laminar surface of evaluating oneself super-hydrophobic in; Surface transparent matter material and good fraction of coverage are provided, also as the carrier of coating surface fluorine monomer; The active fluorine monomer that is adopted, the unit molecule fluorine content is big, and surface energy is extremely low, is enriched in the surface in the solidification process, and crosslinked with generations such as the inner PUA of system, reactive thinners, thereby forms stable, fine and close super hydrophobic surface.Break away from the limitation thinking that traditional self stratifying coating uses the physical blending method mostly;
(3) in the process that makes up the coating surface micro nano structure; Further its kinetics is studied; Gradient dispersion phenomenon to modification low surface energy nanoparticle possibly occur in the paint solidification process is studied and is used, and has further filled up present domestic deficiency to correlative study in the micro-nano surperficial building process;
(4) the project UV cured polyurethane acrylate super hydrophobic coating studying and prepare has been filled up domestic and international blank field, and range of application can expand to relevant special industry, and market outlook are wide; Accelerated the coating material solidified development of China UV, and to the speciality coating development research basis and theoretical basis are provided for it;
(5) through introducing the monomer of special construction, make coating curing after, finger is by getting on not stay fingerprint trace.
Embodiment
For the ease of those skilled in the art's understanding, below in conjunction with the present invention being done further description.
A kind of UV of present embodiment solidifies super-hydrophobic fingerprint-resistant coating, and this coating is by polyurethane acrylate resin, acrylate resin, active fluorine monomer, silicone resin and modified Nano SiO
2Form; Described UV cured coating film is made up of urethane acrylate oligomer, reactive thinner, light trigger and auxiliary agent.This coating each component concentration by mass percentage is: the polyurethane acrylate resin consumption is 25%, acrylate resin 15%, active fluorine monomer 5%, silicone resin 10%, modified manometer silicon dioxide 4%, reactive thinner 7%, light trigger 1%, auxiliary agent 33%.UV solidify super-hydrophobic fingerprint-resistant coating adopt highly active PUA oligopolymer, reactive thinner, and light trigger etc. to process UV coating material solidified, add the monomer opposing fingerprint trace of special construction; On this basis, introduce active fluorine monomer, silicone resin etc. and form surface compacts, stable, thereby reach the automatically cleaning effect from the hydrophobic varnish of layering; And through modified Nano SiO
2Adopt self-assembling technique to make up the UV that surface micronano structure makes it to become excellent performance and solidify super-hydrophobic fingerprint-resistant coating.
Described urethane acrylate oligomer is generated by hexamethylene diisocyanate trimer and Propylene glycol monoacrylate reaction, and this urethane acrylate oligomer is a small molecular weight three-functionality-degree urethane acrylate oligomer.Because the photopolymerization reaction of oligopolymer urethane acrylate (PUA) is active in epoxy acrylate; Curing speed is slow, viscosity is high; Greatly limited it and done the application of oligopolymer, the excellent properties of urethane can not well be used in UV is coating material solidified.So; Urethane acrylate oligomer of the present invention selects for use the reaction of hexamethylene diisocyanate trimer (HDI tripolymer) and Propylene glycol monoacrylate (HPA) to generate small molecular weight three-functionality-degree urethane acrylate (PUA) oligopolymer, each molecule contains six polarity carbamate groups and three active unsaturated double-bonds, when having increased coating to the sticking power of base material; Greatly increased laser curing velocity; Overcome the drawback of conventional P UA oligopolymer, kept the excellent properties that urethane itself is had, enlarged PUA solidifies oligopolymer as UV range of application; Adopt the monomer of special construction to participate in polymerization, make the very anti-fingerprint of coatingsurface.
Described acrylate resin is synthesized by TEB 3K, methyl acrylate, Bing Xisuandingzhi, and this acrylate resin is a LV high-solid content acrylic acid ester resin.Select TEB 3K (MMA), methyl acrylate (MA), Bing Xisuandingzhi synthetic LV high-solid content acrylic acid ester resins such as (BA) for use; Institute's synthetic resin has low surface energy; Except performances such as the sticking power of UV cured coating film, weathering resistance, chemical resistance are improved; Regulate the second-order transition temperature (Tg) and the film forming properties of coating; Form self stratifying coating with UV curing system cured process in addition, the low surface energy polyacrylate resin is that coating surface forms low surface energy structures.
Described light trigger is by 1-hydroxy cyclohexyl phenylketone and 2,4, and these two kinds of light triggers of 6-trimethylbenzoyl diphenyl phosphine oxide are formed.Light trigger can produce radical as photodestruciton type composite initiation system in the broad ultraviolet region, accomplish the fast setting of system; Select the reactive thinner of different functionality for use, in the photocuring process, cooperate PUA oligopolymer generation crosslinking reaction, when playing diluting effect, regulate the second-order transition temperature and the performance of solidifying back coating.
Described active fluorine monomer is high reactivity, fluorine content height and has lower surfactivity and have low surface-active fluorine monomer.The fluorine monomer of employing low surface energy and silicone resin etc.; The UV curing system is in solvent evaporates, drying and solidification process; Be separated with common generation of acrylate resin, surfactivity can be automatically migrated to film coated surface by low material, wherein silicone resin film forming automatically; Active fluorine monomer migrate to the surface and in the UV solidification process with system oligopolymer, reactive thinner take place crosslinked, thereby form fine and close, stable low surface energy hydrophobic structure.
Use Fourier infrared spectrograph (FTIR), DSC (DSC), UV such as sign such as thermal analyzer (TG) instrument of etc.ing solidifies the performances such as second-order transition temperature and thermotolerance of composition and the paint film of super-hydrophobic fingerprint-resistant coating.Use paint film spreader uniform coating and solidify, the varnish optical property is detected through instruments such as photoelectric glossmeter, determination of light transmittance appearance; Through instrument test paint film physicalies such as pencil hardness scratching instrument, impact tester, tensile shear appearance; Detect the chemically-resistant and the corrosive nature of paint film through GB and pertinent instruments; Through water contact angle appearance test coating surface hydrophobic performance.Through test, UV solidifies super-hydrophobic fingerprint-resistant coating and has good optical performance, physics and chemical property, formation surface water droplet contact angle>=150 °, tumbles the ultra-hydrophobicity of angle≤5 °, breaks through light transmission, from the performance of layering technology, micro nano structure.
Embodiment 2
This enforcement 2 is on the basis of embodiment 1, to change; Be specially each components contents difference that UV solidifies super-hydrophobic fingerprint-resistant coating; This coating each component concentration by mass percentage is: polyurethane acrylate resin 36.5%, acrylate resin 12%, active fluorine monomer 4%, silicone resin 8%; Modified manometer silicon dioxide 3%, reactive thinner 6%, light trigger 0.5%, auxiliary agent 30%.
Embodiment 3
This enforcement 3 is on the basis of embodiment 1, to change; Be specially each components contents difference that UV solidifies super-hydrophobic fingerprint-resistant coating; This coating each component concentration by mass percentage is: polyurethane acrylate resin 50.45%, acrylate resin 10%, active fluorine monomer 0.5%, silicone resin 5%; Modified manometer silicon dioxide 1%, reactive thinner 5%, light trigger 0.05%, auxiliary agent 28%.
Above-described embodiment of the present invention does not constitute the qualification to protection domain of the present invention.Any modification of within spirit of the present invention and principle, being done, be equal to replacement and improvement etc., all should be included in claim protection domain of the present invention.
Claims (8)
1. a UV solidifies super-hydrophobic fingerprint-resistant coating, it is characterized in that: this coating is by polyurethane acrylate resin, acrylate resin, active fluorine monomer, silicone resin and modified Nano SiO
2Form; Described UV cured coating film is made up of urethane acrylate oligomer, reactive thinner, light trigger and auxiliary agent.
2. UV according to claim 1 solidifies super-hydrophobic fingerprint-resistant coating; It is characterized in that: this coating each component concentration by mass percentage is: polyurethane acrylate resin 25-50.45%, acrylate resin 10-15%, active fluorine monomer 0.5-5%, silicone resin 5-10%; Modified manometer silicon dioxide 1-4%; Reactive thinner 5-7%, light trigger 0.05-1%, auxiliary agent 28-33%.
3. UV according to claim 1 solidifies super-hydrophobic fingerprint-resistant coating; It is characterized in that: described urethane acrylate oligomer is generated by hexamethylene diisocyanate trimer and Propylene glycol monoacrylate reaction, and this urethane acrylate oligomer is a small molecular weight three-functionality-degree urethane acrylate oligomer.
4. UV according to claim 1 solidifies super-hydrophobic fingerprint-resistant coating; It is characterized in that: described acrylate resin is synthesized by TEB 3K, methyl acrylate, Bing Xisuandingzhi, and this acrylate resin is a LV high-solid content acrylic acid ester resin.
5. UV according to claim 1 solidifies super-hydrophobic fingerprint-resistant coating, it is characterized in that: described acrylate resin is synthesized by TEB 3K, Bing Xisuandingzhi, vinylbenzene, vinyl cyanide.
6. UV according to claim 1 solidifies super-hydrophobic fingerprint-resistant coating, it is characterized in that: described light trigger is by 1-hydroxy cyclohexyl phenylketone and 2,4, and these two kinds of light triggers of 6-trimethylbenzoyl diphenyl phosphine oxide are formed.
7. UV according to claim 1 solidifies super-hydrophobic fingerprint-resistant coating, it is characterized in that: described active fluorine monomer is high reactivity, fluorine content height and has lower surfactivity and have low surface-active fluorine monomer.
8. the preparation method of solidifying super-hydrophobic fingerprint-resistant coating according to each described UV of claim 1-7, it is characterized in that: this preparing method's step is:
(1) adopt hexamethylene diisocyanate trimer and Propylene glycol monoacrylate under catalyzer and stopper effect, to carry out single step reaction, generation has the three-functionality-degree urethane acrylate oligomer of high reaction activity small molecular weight, solidifies oligopolymer as UV; The reactive thinner that adds different functionality, the performance of regulating the active of photocuring reaction and solidifying the back paint film; Add 1-hydroxy cyclohexyl phenylketone and 2,4,6-trimethylbenzoyl diphenyl phosphine oxide is as light trigger; Introduce acrylate resin and improve curing performance, and regulate the second-order transition temperature and the film-forming properties of paint film;
(2) adopt high reactivity, fluorine content is high and the silicone resin that has lower surfactivity and have low surface-active fluorine monomer, a high heat resistance as the low surface energy material; In solvent evaporates, drying and solidification process; Be automatically migrated to coatingsurface, it is crosslinked through UV curing coatingsurface fluorine monomer and the inner oligopolymer of system, reactive thinner to be taken place, in addition; Acrylate resin, silicone resin be film forming automatically, thereby makes coatingsurface form densification, stable low surface energy hydrophobic structure;
(3) employing is carried out chemically modified and parcel to nanoparticle surface, forms dewatering nano SiO
2, through the nanometer SiO after the modification
2The surface is than strong-hydrophobicity and has the functional functional group that can react, adds in the UV curing system, makes up the surperficial micro nano structure of varnish with secondary composite structure and the surface hydrophobicity that it was had, and makes UV and solidifies super-hydrophobic fingerprint-resistant coating.
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Application publication date: 20120919 |