CN105176296A - High-temperature resistant coating based on polysilsesquioxane modification and application thereof - Google Patents
High-temperature resistant coating based on polysilsesquioxane modification and application thereof Download PDFInfo
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Abstract
The invention discloses a high-temperature resistant coating based on polysilsesquioxane modification and an application thereof. In the embodiments, the high-temperature resistant coating comprises components in mass of 15%-30% of modified organic resin, 25%-50% of modified pigment, 1%-5% of dispersing agent, 0.1%-3% of flatting agent, 0.2%-3% of compound additive and 3%-20% of solvent. According to the high-temperature resistant coating based on polysilsesquioxane modification and the application thereof, polysilsesquioxane is used as a modifying agent for modifying film-forming resin and pigment, the quality of the high-temperature resistant coating can be further improved, the comprehensive performance of the high-temperature resistant coating is effectively improved, and particularly, the hardness, the stability, the scratch resistance, the compactness and the crack resistance of the high-temperature resistant coating under the high temperature condition are improved greatly.
Description
Technical field
The invention belongs to Material Field, relate to a special functional coating, be specifically related to a kind of high-temperature resistant coating based on polysilsesquioxane modification and application thereof.
Background technology
High-temperature resistant coating generally refers to that heatproof is more than 200 DEG C, paint film nondiscoloration, does not come off, and still can keep the coating of suitable physical and mechanical properties, can make the special functional coating that protected object can normally play a role in hot environment.Along with developing rapidly of the industries such as Aeronautics and Astronautics, automobile and civilian household electrical appliance, the use properties for metal or glass material requires more and more higher, and high-temperature resistant coating also more and more comes into one's own, and can obtain using more and more widely.Due to the environment for use requirement of harshness, not only need coating can use under higher use temperature and more harsh environment, also require that coating at high temperature has good hardness, tack, wear resistance etc. simultaneously.And existing high-temperature resistant coating, the shortcomings such as under the high temperature conditions, especially more than in the environments for use of 200 DEG C, ubiquity sticking power is bad, easily be full of cracks, efflorescence, and hardness decline is fast.
Summary of the invention
For the deficiencies in the prior art, the object of the present invention is to provide a kind of high-temperature resistant coating based on polysilsesquioxane modification and application thereof.
For realizing aforementioned invention object, the technical solution used in the present invention comprises:
Based on a high-temperature resistant coating for polysilsesquioxane modification, comprise:
Modified organic resin, is selected from by the organic resin of polysilsesquioxane modification,
Modification color stuffing, comprises by the pigment of polysilsesquioxane modification and/or filler,
The film coalescence aid adding or do not add can be selected,
And, the solvent adding or do not add can be selected;
Further, at least one component in described high-temperature resistant coating is fluid, and this at least one component can be uniformly mixed to form the described high-temperature resistant coating in flow-like with all the other components in this high-temperature resistant coating.
Among some embodiments, described high-temperature resistant coating comprises 15wt% ~ 30wt% modified organic resin.
Preferably, described organic resin comprises any one or the two or more combinations in polyether-ether-ketone resin, fluorocarbon resin, polyphenylene sulfide, silicone resin, polyimide resin.
Described high-temperature resistant coating comprises 25wt% ~ 50wt% modification color stuffing.
Preferably, described pigment comprises any one or the two or more combinations in carbon black, cobalt black, cobalt blue, cobalt green, copper-chrome black, titanium nickel yellow, titanium white, cadmium red, titanium chromium palm fibre, red iron oxide, zirconium white.
Preferably, described filler comprises any one or the two or more combinations in calcium carbonate, kaolin, talcum powder, calcium sulfate, barium sulfate, wollastonite, mica, silica powder.
Preferably, the mass ratio of described pigment and filler is 2:1 ~ 1:3.
Among some embodiments, described film coalescence aid comprises any one or two or more combinations in dispersion agent, flow agent, composite assistant.
Preferably, described high-temperature resistant coating comprises: dispersion agent 1wt% ~ 5wt%, flow agent 0.1wt% ~ 3wt%, composite assistant 0.2wt% ~ 3wt%.
Wherein, dispersion agent (Dispersant) to reduce the material that in dispersion system, solid or liquid particle are assembled, such as can be selected from a kind of interfacial agent simultaneously in molecule with lipophilicity and wetting ability two kinds of opposite nature, its can homogeneous dispersion those be difficult to be dissolved in the inorganic of liquid, the solid of pigment dyestuff and liquid particle, also can prevent the sedimentation of particle and cohesion simultaneously and form stable suspensoid.
Preferably, described dispersion agent includes but not limited to polyamide-based, fatty acid polyglycol alkoxide, the commercially available general types such as silicone based, as BYK-164, BYK-174 (German Bi Ke company), any one or two or more combinations in Silok-714 (Guangzhou Si Luoke Chemical Co., Ltd.), but be not limited thereto.
Wherein, flow agent (Levelingagent), flow agent is a kind of conventional coatings additive(s), and it can impel coating in drying and forming-film process, form smooth, smooth, a uniform film.Effectively can reduce and cover with paint, lacquer, colour wash, etc. liquid surface tension, improve a class material of its levelling property and homogeneity.
Described flow agent includes but not limited to the commercially available general types such as esters of acrylic acid, urea-formaldehyde resin class, silicone resin class, as BYK-313, BYK-300 (German Bi Ke company), DC-57 (Dow corning company), Silok-810 (Guangzhou Si Luoke Chemical Co., Ltd.).
Known to the preferred industry of described assistant agent, to be usually used in high-temperature resistant coating suitable flow agent, defoamer, thickening material and all the other secondary solvents etc., and be not limited thereto.
Preferably, described composite assistant comprises mass ratio is the polymer adhesion promoter of the band epoxy group(ing) of 1:1 ~ 1:5 and the silane coupling agent being with amino or epoxy group(ing).
Among some embodiments, the described high-temperature resistant coating based on polysilsesquioxane modification also comprises 3wt% ~ 20wt% solvent.
Preferably, described solvent comprises any one or two or more combinations in benzene,toluene,xylene, normal hexane, dioxane, DBE (high boiling solvent mixed dibasic acid ester), petroleum naphtha, ethyl acetate or N-BUTYL ACETATE, but is not limited thereto.
Among some embodiments, the chemical general formula of described polysilsesquioxane is (RSiO
3/2) n; Wherein, if R is reactive group, then described R base comprises any one or the two or more combinations in thiazolinyl, epoxy group(ing) or amino; If R is inertia group, then described R base comprises any one or the two or more combinations in the alkyl of C1 ~ C4, alkylene or aryl; N is the arbitrary integer in 20 ~ 40.
Among some comparatively specific embodiment, the preparation method of described modified organic resin comprises: by polysilsesquioxane and organic resin in mass ratio 1:5 ~ 1:10 feed intake, and add catalyzer and organic solvent, under 45 ~ 85 DEG C of conditions, react 2 ~ 4h after Homogeneous phase mixing, obtain the organic resin containing silsesquioxane modification.
Preferably, the consumption of described catalyzer is 0.15% ~ 0.3% of this modified organic resin preparation feedback system total mass.
Preferably, the consumption of described organic solvent is 20% of organic resin quality.
Preferably, described catalyzer comprises any one or two or more combinations in tetramethyl-oxyammonia, tetrabutylammonium hydroxide amine, 4-butyl-phosphonium acetate, trolamine, triphenyl phosphorus, benzyldimethylamine, dibutyltin dilaurate, triethylenediamine, but is not limited thereto.
Preferably, described organic solvent comprises toluene and/or dimethylbenzene, but is not limited thereto.
Among some embodiments, the preparation method of described modification color stuffing comprises:
By pigment and fillers dispersed in coupling agent solution, and be return stirring 0.5h ~ 2h under the condition of 40 DEG C ~ 80 DEG C in temperature, then isolate rough color stuffing again polysilsesquioxane, rough color stuffing, organic solvent to be mixed by the mass ratio of 1:5:6 ~ 1:10:11, be back flow reaction 0.5h ~ 2h under the condition of 40 DEG C ~ 85 DEG C afterwards in temperature, obtained described modification color stuffing.
Preferably, described coupling agent solution is selected from the ethanolic soln that concentration is 1wt% ~ 10wt% coupling agent.
Preferably, described coupling agent comprises any one or two or more combinations in KH550, KH560, KH570 or KH590, but is not limited thereto.
Preferably, described organic solvent comprises toluene and/or dimethylbenzene.
The invention allows for the described application based on the high-temperature resistant coating of polysilsesquioxane modification.
Such as, in some embodiments provide a kind of high-temperaure coating, solidify to form primarily of the described high-temperature resistant coating based on polysilsesquioxane modification.
Such as, in some embodiments provide a kind of preparation method of high-temperaure coating, comprising: the described high-temperature resistant coating based on polysilsesquioxane modification is coated on base material, then be solidify to form described coating under the condition of 150 DEG C ~ 300 DEG C in temperature.
Such as, in some embodiments provide a kind of device, comprise described high-temperaure coating.
The described high-temperature resistant coating based on polysilsesquioxane modification can widespread use in the industries such as aviation, automobile or civil electric appliance.
The present invention carries out physical and chemical modified as properties-correcting agent to film-forming resin and color stuffing by using polysilsesquioxane, utilizes the chemical reaction that polysilsesquioxane and organic resin and inorganic color stuffing surface occur.On the one hand, the problem of hardness rapid drawdown under coating high-temp can be improved by introducing the polysilsesquioxane with rigidity three-dimensional arrangement, substantially increase the hardness of existing high-temperature resistant coating, solve the problem that its coating scratch resistance capability is low and existing high-temperature resistant coating high temperatures is bad.On the other hand, polysilsesquioxane and inorganic color stuffing surface group react, and effectively inhibit the reunion of color stuffing particle, improve the dispersiveness of color stuffing.Especially, organic resin and polysilsesquioxane generation chemical crosslink reaction, also the consistency between resin and inorganic color stuffing is substantially increased, thus improve the compactness of coating further, and then improve coating splitting resistance at high temperature, the problem cracked under effectively reducing coating high-temp.
In a word, compared with prior art, advantage of the present invention comprises: the quality that can promote high-temperature resistant coating further, and effectively improve the over-all properties of coating, particularly significantly can promote coating hardness under the high temperature conditions, stability, scratch resistance capability, compactness and anti-cracking performance, therefore have a good application prospect.
Embodiment
In view of deficiency of the prior art, inventor, through studying for a long period of time and putting into practice in a large number, is proposed technical scheme of the present invention.To be further explained this technical scheme, its implementation process and principle etc. in conjunction with some embodiments as follows.
Embodiment 1
(1) by TMS cage type polysilsesquioxane and polyether-ether-ketone resin in mass ratio 1:5 feed intake in reactor, and the catalyzer tetramethyl-oxyammonia added by reaction system total mass 0.15% and the toluene accounting for resin total mass 20%, Homogeneous phase mixing; Under 45 DEG C of conditions, react 4h, obtain the organic resin containing silsesquioxane modification;
(2) cobalt black, mica are placed in respectively containing 1% in the ethanolic soln of (if not following special instruction, being then wt%) coupling agent KH550, are return stirring 0.5h under the condition of 40 DEG C in temperature, cool afterwards, filter, dry for standby.
(3) gained face, filler, toluene in TMS cage type polysilsesquioxane and step (2) are mixed in the ratio of 1:5:6, under temperature is 40 DEG C of conditions, carries out back flow reaction 2h, cools for subsequent use afterwards.
(4) adhesion promoter 7130 of band epoxy group(ing), Silane coupling agent KH550, dimethylbenzene are mixed in the ratio (mass ratio) of 1:1:1, prepare composite assistant.
(5) by following formulated high-temperature resistant coating, dispersing and mixing is even: modified organic resin 15%; Modification color stuffing 45%; BYK-164 dispersion agent 5%; BYK-313 flow agent 1%; Composite assistant 1%; Toluene 10%.This coating is applied on base material and solidifies 1h 250 DEG C time, and then the hardness measured after 400 DEG C of calcining 1h is 4H.Coating has a small amount of crackle under SEM Electronic Speculum, and length is between 1 ~ 3 micron.
Embodiment 2
(1) by tetramethyl-ammonium cage type polysilsesquioxane and fluorocarbon resin in mass ratio 1:7 feed intake in reactor, and add by reaction system total mass 0.2% catalyzer tetrabutylammonium hydroxide amine and account for the dimethylbenzene of resin total mass 20%, Homogeneous phase mixing; Under 55 DEG C of conditions, react 2.5h, obtain the organic resin containing silsesquioxane modification;
(2) copper-chrome black, barium sulfate are placed in respectively the ethanolic soln containing 3% coupling agent KH560, are return stirring 1h under the condition of 50 DEG C in temperature, cool afterwards, filter, dry for standby.
(3) gained face, filler, dimethylbenzene in tetramethyl-ammonium cage type polysilsesquioxane and step (2) are mixed in the ratio of 1:6:8, under temperature is 50 DEG C of conditions, carries out back flow reaction 1.5h, cools for subsequent use afterwards.
(4) adhesion promoter HSM-900, the silane coupling agent KH560 of band epoxy group(ing), dimethylbenzene are mixed in the ratio of 1:3:1, prepare composite assistant.
(5) by following formulated high-temperature resistant coating, dispersing and mixing is even: modified organic resin 20%; Modification color stuffing 50%; BYK-174 dispersion agent 3%; BYK-300 flow agent 0.1%; Composite assistant 0.2%; Ethyl acetate 8%.This coating is applied on base material and solidifies 1h 150 DEG C time, and then the hardness measured after 400 DEG C of calcining 1h is 3H.Coating almost flawless under SEM Electronic Speculum.
Embodiment 3
(1) by dimethyl diphenyl-methyl ethylene polysilsesquioxane and silicone resin in mass ratio 1:8 feed intake in reactor, and the catalyzer trolamine added by reaction system total mass 0.25% and the toluene accounting for resin total mass 20%, Homogeneous phase mixing; Under 60 DEG C of conditions, react 2.5h, obtain the organic resin containing silsesquioxane modification;
(2) red iron oxide, silica powder are placed in respectively the ethanolic soln containing 5% coupling agent KH570, are return stirring 1h under the condition of 60 DEG C in temperature, cool afterwards, filter, dry for standby.
(3) gained face, filler, dimethylbenzene in dimethyl diphenyl-methyl ethylene polysilsesquioxane and step (2) are mixed in the ratio of 1:8:9, under temperature is 65 DEG C of conditions, carries out back flow reaction 1.5h, cools for subsequent use afterwards.
(4) the adhesion promoter D-6040 of band epoxy group(ing), Silane coupling agent KH550, dimethylbenzene are mixed in the ratio of 1:5:1, prepare composite assistant.
(5) by following formulated high-temperature resistant coating, dispersing and mixing is even: modified organic resin 25%; Modification color stuffing 30%; Silok-714 dispersion agent 1%; DC-57 flow agent 1.5%; Composite assistant 0.8%; N-BUTYL ACETATE 3%.This coating is applied on base material and solidifies 1h 300 DEG C time, and then the hardness measured after 400 DEG C of calcining 1h is 4H.Coating is flawless under SEM Electronic Speculum.
Embodiment 4
(1) by dimethylsilyl cage type polysilsesquioxane and polyimide resin in mass ratio 1:10 feed intake in reactor, and add and account for the toluene of resin total mass 10% and the dimethylbenzene of 10% by the catalyzer triethylenediamine neutralization of reaction system total mass 0.15%; Under 80 DEG C of conditions, react 2h, obtain the organic resin containing silsesquioxane modification;
(2) zirconium white, mica are placed in respectively the ethanolic soln containing 8% coupling agent KH590, are return stirring 0.5h under the condition of 80 DEG C in temperature, cool afterwards, filter, dry for standby.
(3) gained color stuffing, toluene solvant in dimethylsilyl cage type polysilsesquioxane and step (2) are mixed in the ratio of 1:10:11, under temperature is 50 DEG C of conditions, carries out back flow reaction 2h, cools for subsequent use afterwards.
(4) adhesion promoter D-6040, the silane coupling agent KH560 of band epoxy group(ing), dimethylbenzene are mixed in the ratio of 1:2:1, prepare composite assistant.
(5) by following formulated high-temperature resistant coating, dispersing and mixing is even: modified organic resin 30%; Modification color stuffing 25%; BYK-174 dispersion agent 4%; Silok-8100 flow agent 3%; Composite assistant 3%; Petroleum naphtha 20%.This coating is applied on base material and solidifies 1h 200 DEG C time, and then the hardness measured after 400 DEG C of calcining 1h is 3H.Coating is flawless under SEM Electronic Speculum.
Comparative example 1:
Carry out being mixed with high-temperature resistant coating according to the formula of step (5) in above-mentioned 4 embodiments respectively, but the resin used and color stuffing are all the raw material without polysilsesquioxane modification, afterwards coating is applied to according to after solidification value solidification in embodiment on base material, then the hardness measured after 400 DEG C of calcining 1h is all less than or equal to 1H.Coating crackle under SEM Electronic Speculum is more, and length is all more than 10 microns.
Comparative example 2:
Carry out being mixed with high-temperature resistant coating according to the formula of step (5) in above-mentioned 4 embodiments respectively, but use the resin through polysilsesquioxane modification, and color stuffing is unmodified, afterwards coating is applied to according to after solidification value solidification in embodiment on base material, then the hardness measured after 400 DEG C of calcining 1h is 2H, 1H, 2H, 1H respectively.Coating has comparatively multiple cracks under SEM Electronic Speculum, and length is between 3 ~ 9 microns.
Comparative example 3:
Carry out being mixed with high-temperature resistant coating according to the formula of step (5) in above-mentioned 4 embodiments respectively, but use the color stuffing through polysilsesquioxane modification, and resin non-modified, afterwards coating is applied to according to after solidification value solidification in embodiment on base material, then the hardness measured after 400 DEG C of calcining 1h is 1H, 1H, 2H, 1H respectively.Coating has comparatively multiple cracks under SEM Electronic Speculum, and length is between 3 ~ 9 microns.
Under the hardness value after the high-temperature calcination carried out above and high temperature, crack situation, adopt high-temperature resistant coating prepared by the resin after by process and color stuffing, its performance is obviously promoted.
It should be noted that, as above the various product that adopts of embodiment and correlation parameter, various reaction partner and processing condition are all comparatively typical examples, but verify through inventor's lot of experiments, also be all applicable in other listed above dissimilar reaction partner and other processing condition etc., and also all attainable cost invent the technique effect claimed.
Should be appreciated that above-described embodiment is only and technical conceive of the present invention and feature are described, its object is to person skilled in the art can be understood content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences done according to spirit of the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (10)
1., based on a high-temperature resistant coating for polysilsesquioxane modification, it is characterized in that comprising:
Modified organic resin, is selected from by the organic resin of polysilsesquioxane modification,
Modification color stuffing, comprises by the pigment of polysilsesquioxane modification and/or filler,
The film coalescence aid adding or do not add can be selected,
And, the solvent adding or do not add can be selected;
Further, at least one component in described high-temperature resistant coating is fluid, and this at least one component can be uniformly mixed to form the described high-temperature resistant coating in flow-like with all the other components in this high-temperature resistant coating.
2. the high-temperature resistant coating based on polysilsesquioxane modification according to claim 1, is characterized in that:
Described high-temperature resistant coating comprises 15wt% ~ 30wt% modified organic resin;
Preferably, described organic resin comprises any one or the two or more combinations in polyether-ether-ketone resin, fluorocarbon resin, polyphenylene sulfide, silicone resin, polyimide resin;
And/or described high-temperature resistant coating comprises 25wt% ~ 50wt% modification color stuffing;
Preferably, described pigment comprises any one or the two or more combinations in carbon black, cobalt black, cobalt blue, cobalt green, copper-chrome black, titanium nickel yellow, titanium white, cadmium red, titanium chromium palm fibre, red iron oxide, zirconium white;
Preferably, described filler comprises any one or the two or more combinations in calcium carbonate, kaolin, talcum powder, calcium sulfate, barium sulfate, wollastonite, mica, silica powder;
Preferably, the mass ratio of described pigment and filler is 2:1 ~ 1:3.
3. the high-temperature resistant coating based on polysilsesquioxane modification according to claim 1, is characterized in that:
Described film coalescence aid comprises any one or two or more combinations in dispersion agent, flow agent, composite assistant;
Preferably, described high-temperature resistant coating comprises: dispersion agent 1wt% ~ 5wt%, flow agent 0.1wt% ~ 3wt%, composite assistant 0.2wt% ~ 3wt%;
Preferably, described dispersion agent comprises polyamide-based, fatty acid polyglycol alkoxide or silicone based dispersion agent;
Preferably, described flow agent comprises esters of acrylic acid, urea-formaldehyde resin class or silicone resin class flow agent;
Preferably, described composite assistant comprises mass ratio is the polymer adhesion promoter of the band epoxy group(ing) of 1:1 ~ 1:5 and the silane coupling agent being with amino or epoxy group(ing).
4., according to claim 1 based on the high-temperature resistant coating of polysilsesquioxane modification, characterized by further comprising 3wt% ~ 20wt% solvent;
Preferably, described solvent comprises any one or the two or more combinations in benzene,toluene,xylene, normal hexane, dioxane, DBE, petroleum naphtha, ethyl acetate or N-BUTYL ACETATE.
5., according to claim 1 based on the high-temperature resistant coating of polysilsesquioxane modification, it is characterized in that the chemical general formula of described polysilsesquioxane is (RSiO
3/2) n; Wherein, if R is reactive group, then described R base comprises any one or the two or more combinations in thiazolinyl, epoxy group(ing) or amino; If R is inertia group, then described R base comprises any one or the two or more combinations in the alkyl of C1 ~ C4, alkylene or aryl; N is the arbitrary integer in 20 ~ 40.
6. according to claim 1,2 or 5 based on the high-temperature resistant coating of polysilsesquioxane modification, it is characterized in that the preparation method of described modified organic resin comprises: by polysilsesquioxane and organic resin in mass ratio 1:5 ~ 1:10 feed intake, and add catalyzer and organic solvent, under 45 ~ 85 DEG C of conditions, react 2 ~ 4h after Homogeneous phase mixing, obtain the organic resin containing silsesquioxane modification;
Preferably, the consumption of described catalyzer is 0.15% ~ 0.3% of this modified organic resin preparation feedback system total mass;
Preferably, the consumption of described organic solvent is 20% of organic resin quality;
Preferably, described catalyzer comprises any one or the two or more combinations in tetramethyl-oxyammonia, tetrabutylammonium hydroxide amine, 4-butyl-phosphonium acetate, trolamine, triphenyl phosphorus, benzyldimethylamine, dibutyltin dilaurate, triethylenediamine;
Preferably, described organic solvent comprises toluene and/or dimethylbenzene.
7., according to claim 1 based on the high-temperature resistant coating of polysilsesquioxane modification, it is characterized in that the preparation method of described modification color stuffing comprises:
By pigment and fillers dispersed in coupling agent solution, and be return stirring 0.5h ~ 2h under the condition of 40 DEG C ~ 80 DEG C in temperature, then isolate rough color stuffing again polysilsesquioxane, rough color stuffing, organic solvent to be mixed by the mass ratio of 1:5:6 ~ 1:10:11, be back flow reaction 0.5h ~ 2h under the condition of 40 DEG C ~ 85 DEG C afterwards in temperature, obtained described modification color stuffing;
Preferably, described coupling agent solution is selected from the ethanolic soln that concentration is 1wt% ~ 10wt% coupling agent;
Preferably, described coupling agent comprises any one or the two or more combinations in KH550, KH560, KH570 or KH590;
Preferably, described organic solvent comprises toluene and/or dimethylbenzene.
8. a high-temperaure coating, solidify to form primarily of the high-temperature resistant coating based on polysilsesquioxane modification according to any one of claim 1-7.
9. the preparation method of a high-temperaure coating, it is characterized in that comprising: the high-temperature resistant coating based on polysilsesquioxane modification according to any one of claim 1-7 is coated on base material, then be solidify to form described coating under the condition of 150 DEG C ~ 300 DEG C in temperature.
10. a device, is characterized in that comprising high-temperaure coating according to claim 8.
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