CN100554344C - A kind of anti-ultraviolet paint composition and uvioresistant film - Google Patents
A kind of anti-ultraviolet paint composition and uvioresistant film Download PDFInfo
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- CN100554344C CN100554344C CNB2007100203307A CN200710020330A CN100554344C CN 100554344 C CN100554344 C CN 100554344C CN B2007100203307 A CNB2007100203307 A CN B2007100203307A CN 200710020330 A CN200710020330 A CN 200710020330A CN 100554344 C CN100554344 C CN 100554344C
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Abstract
The invention provides a kind of anti-UV coating composition that comprises inorganic particles, organic filler and resin, this coating composition can be coated on the base material, makes base material have good anti-UV effect.Simultaneously, the present invention also provides a kind of anti-UV film, its at least one mask that comprises a base material and this base material has at least one deck by the formed anti-UV layer of the anti-UV coating composition of the present invention, this film can strengthen briliancy, has good weathering resistance, and have the ultraviolet character of absorption, and can effectively solve the problem of base material yellow, can play good effect for backlight modules such as LCD.
Description
Technical field
The present invention relates to coating composition, relate in particular to a kind of coating composition with anti-ultraviolet property, and the film that comprises the uvioresistant coating, coating processing and applied technical field thereof belonged to.
Background technology
Backlight module (back light module) is one of key components and parts of LCD panel.Because liquid crystal itself can't be luminous voluntarily, liquid crystal panel is even so the backlight module major function provides, the light source of high brightness, its ultimate principle is with point or linear light sources commonly used, see through the area source product that succinct effectively optical facilities change into high brightness, briliancy homogeneous, provide product required backlight by this, make its normally show image.Under the current state, backlight module is quite big for the manufacturing cost and the using character influence of liquid-crystal display.
Comparatively general on the market backlight module is classified according to the position of fluorescent tube, mainly is divided into side type structure and straight-down negative structure.In general side type backlight module, reflectance coating is arranged on the bottom of light guiding plate usually, and the luminous reflectance that is used for spilling from the bottom surface returns light guiding plate, prevents that light source from leaking outside, to increase the service efficiency of light.And in direct type backlight module, reflectance coating then is arranged at the lamp box lower surface or pastes thereon, with the light beam of fluorescent tube direct irradiation and through the diffuser plate beam reflected from the lamp box bottom reflected back diffuser plate once more, and then be utilized.Generally speaking, the function of reflectance coating in these two kinds of structures all is the service efficiency that promotes light source.
Yet the light that general fluorescent tube is launched contains ultraviolet ray (UV), and ultraviolet ray easily makes the macromolecule resin yellow in the blooming, causes the reflection of light rate to descend, and luminous reflectance look aberration occurs.According to the knowledge of the applicant, all there is above-mentioned deficiency to a certain extent in existing various LCD panels, and just because of this, research and development are applicable to the more superior anti-ultraviolet paint of performance of backlight module blooming, have become important technology problem in the industry.
Summary of the invention
First purpose of the present invention provides a kind of anti-ultraviolet paint composition that comprises inorganic particles, organic filler and macromolecule resin.
Another object of the present invention provides a kind of film, and at least one mask that it comprises a base material and this base material has at least one deck by the formed uvioresistant coating of anti-ultraviolet paint composition.
For realizing first purpose of the present invention, a kind of anti-ultraviolet paint composition, comprise inorganic particles and resin, it is characterized in that: also contain organic filler in the middle of this coating composition, described organic filler is different with the specific refractory power of resin, and the absolute value of the difference of both specific refractory poweres is at least 0.07, is at most 0.6.
Further, above-mentioned anti-ultraviolet paint composition, wherein, the specific refractory power of described organic filler is 1.40 to 1.60.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, the particle diameter of described organic filler is 0.1 micron to 10 microns.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, the particle diameter of described organic filler is 1 micron to 5 microns.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, the quality of described organic filler is 1% to 500% of a resin quality.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, the quality of described organic filler is 10% to 300% of a resin quality.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, described organic filler is selected from the group that is made of methacrylic resin, silicone resin and composition thereof.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, described organic filler is a silicone resin.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, described inorganic particulate is selected from the group that is made of zinc oxide, silicon-dioxide, titanium dioxide, zirconium white, aluminum oxide, barium sulfate, lime carbonate and composition thereof.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, described inorganic particulate is selected from the group that is made of zinc oxide, titanium dioxide and composition thereof.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, the particle diameter of described inorganic particulate is 1～1000 nanometer.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, the quality of described inorganic particulate is 0.1% to 100% of a resin quality.
Again further, above-mentioned anti-ultraviolet paint composition, wherein, described resin is selected from the group that is made of acrylic resin, methacrylic resin, polyamide resin, Resins, epoxy, fluoroplast, polyimide resin, polyurethane resin, Synolac, vibrin and composition thereof.
Further, above-mentioned anti-ultraviolet paint composition, wherein, described resin is methacrylic resin or fluoroplast.
Be to realize second purpose of the present invention, a kind of uvioresistant film comprises an optical element, it is characterized in that: the uvioresistant coating that at least one mask of described optical element has one deck at least to be formed by aforementioned coating composition.
Again further, above-mentioned uvioresistant film, wherein, described optical element is reflective substrate or transparent substrate.
Again further, above-mentioned uvioresistant film, wherein, described optical element is the reflective substrate of single or multiple lift structure, records its yellowness index changing value (Δ YI) less than 2 according to ASTM G154 and ASTM E313 standard method.
Again further, above-mentioned uvioresistant film, wherein, described reflective substrate is an expanded plastic, or contains the plastics of particle, or expanded plastic and contain the composition of particle plastics.
Again further, above-mentioned uvioresistant film, wherein, described reflective substrate contains bubble and particle simultaneously.
Again further, above-mentioned uvioresistant film, wherein, the diameter of described bubble and particle is 0.01 micron to 10 microns.
Again further, above-mentioned uvioresistant film, wherein, described particle is organic filler or inorganic particulate.
Again further, above-mentioned uvioresistant film, wherein, described particle is an organic filler, described organic filler is selected from the group that is made of methacrylic resin, amido formate resin, silicone resin and composition thereof.
Again further, above-mentioned uvioresistant film, wherein, described particle is an inorganic particulate, described inorganic particulate is selected from the group that is made of zinc oxide, silicon-dioxide, titanium dioxide, aluminum oxide, calcium sulfate, barium sulfate, lime carbonate and composition thereof.
Again further, above-mentioned uvioresistant film, wherein, the thickness of described optical element is 16 microns to 1000 microns.
Again further, above-mentioned uvioresistant film, wherein, the thickness of described uvioresistant coating is 1 micron to 20 microns.
Again further, above-mentioned uvioresistant film, wherein, the thickness of described uvioresistant coating is 3 microns to 15 microns.
Further, above-mentioned uvioresistant film, wherein, according to ASTM 903-96 standard method, the reflectivity or the penetration coefficient that record this uvioresistant film when wavelength 313nm are lower than 10%, and it is arranged on and is used as reflectance coating or diffusion barrier in the display backlight module.
Description by above technical scheme can be found, outstanding substantive distinguishing features of the present invention is embodied in marked improvement: owing to add the organic filler that has different specific refractory poweres with resin in the middle of coating composition, so when the light from light source enters by the formed coating of the anti-UV coating composition of the present invention, light repeatedly reflects in coating inside, make the travel path of light prolong, easilier contact, absorb ultraviolet effect thereby improve with inorganic particles.This coating composition is coated the optical element surface, but the enhanced film briliancy has good weathering resistance, and have and absorb ultraviolet effect, and can effectively solve the phenomenon of base material yellow, reduce the aberration problem of LCD, reach the purpose that strengthens the liquid-crystal display effect.
Description of drawings
Fig. 1 represents a kind of reflective substrate with known uvioresistant coating.
Fig. 2 represents a kind of reflective substrate that has by the formed uvioresistant coating of coating composition of the present invention.
Fig. 3～6 are for can be used for the synoptic diagram of reflective substrate of the present invention.
Fig. 7 is the light source device synoptic diagram of advertising lamp box.
Fig. 8 is the direct type backlight module schematic representation of apparatus.
Fig. 9 is the side type backlight module schematic representation of apparatus.
Figure 10～Figure 23 represents that successively (QUV weather resistance test machine, setting UVB 313nm fluorescent tube energy is 0.8W/m in the reflected light spectrogram of each test duration point for embodiment 1～8, comparative example 1～6 each diaphragm
2/ nm, envrionment conditions: 60 ℃).
The implication of each Reference numeral is as follows among the figure:
11,21 reflective substrate
12,26 coatings
13,23 light sources
14,24 inorganic particles
22 resins
25 organic fillers
410,510,610,710 reflective substrate
41,51,61,71 first plastic layers
42,52,62,73 second plastic layers
44,54,64 the 3rd plastic layers
43,63,72,74 inorganic particulates
53,65 bubbles
220 direct type backlight modules
230 side type backlight modules
221,231 reflectance coatings
222,232 fluorescent tubes
223 diffuser plates
224,234 diffusion barriers
225,235 condensing films
226, diffusion barrier on 236
233 light guiding plates
237 lampshade reflectance coatings
800 light source devices
80 diaphragm groups
81 diffusion barriers
82 light guiding plates
83 condensing films
84 housings
85 inside casings
Embodiment
At the deficiency that prior art exists, the present inventor develops a kind of uvioresistant (UV) coating composition of novelty through broad research, and this anti-UV coating composition can be coated on the base material, makes base material have good anti-UV effect.This anti-UV coating composition is coated on the optical element surface and the blooming of formation, because of this anti-UV coating composition has the UV receptivity, so can protect blooming not injured by UV-light.This blooming is applied to backlight module, and owing to penetrating or reflex action of light, UV wavelength major part can be absorbed, and therefore also can avoid other blooming of backlight module to influence its optical property because of UV light.
Be applicable to that the resin in the anti-UV coating composition of the present invention there is no particular restriction, includes but not limited to methacrylic resin, polyamide resin, Resins, epoxy, fluoroplast, polyimide resin, polyurethane resin, Synolac, vibrin or its mixture; Be preferably methacrylic resin, fluoroplast or its mixture; Be more preferred from methacrylic resin.Methacrylic resin be with one or more oleic series monomers as the formed macromolecule copolymer resin of polymerized unit, wherein the oleic series monomer has following general formula:
R is hydrogen atom, C in the formula
1-C
18Aliphatic group (aliphatic group) or C
1-C
10Hydroxyalkyl group (hydroxyalkyl).Preferably, R is hydrogen atom, C
1-C
8Alkyl or C
2-C
8Hydroxyalkyl.
Contain the inorganic particles that can absorb UV light in the anti-UV coating composition of the present invention, these inorganic particles be there is no particular restriction, include but not limited to: zinc oxide, silicon-dioxide, titanium dioxide, zirconium white, aluminum oxide, barium sulfate, lime carbonate, or their mixture; Be preferably zinc oxide, titanium dioxide or its mixture, the best is a titanium dioxide.The size of above-mentioned inorganic particles is generally 1～1000 nanometer (nm), is preferably 10～100 nanometers.
The content of the inorganic particles in the anti-UV coating composition of the present invention there is no particular restriction, can be any suitable content.Preferably, this inorganic particles is 0.1～100Wt% with respect to the amount of macromolecule resin, is in particular 1～30Wt%.In addition, generally speaking, if the inorganic particles dispersiveness in the coating composition is not good, easily produce cohesion or sedimentation phenomenon, and then cause prepared crawling and the anti-UV poor effect of filming, therefore, can utilize oxyhydroxide that upgrading is made on the inorganic particles surface and handle, to improve dispersiveness.
Known anti-UV coating composition is to utilize inorganic particles to absorb UV-light.Fig. 1 represents a kind of reflective substrate 11, and its surface has by the formed coating 12 of known anti-UV coating composition.As shown in Figure 1, be incident in base material 11 through coating 12, penetrate through coatings 12 backs via base material 11 reflections again from the light of light source 13.When light process coating 12, can contact also by this with ultraviolet radiation absorption with coating 12 central contained inorganic particles 14.Yet, shorter because of its straightaway path when light passes through by the formed coating of known coating composition, can't carry out more effectively contacting with inorganic particles so that ultraviolet ray is fully absorbed, so anti-UV poor effect.
The anti-UV coating composition of the present invention then comprises at least a specific refractory power organic filler different with resin to address the above problem.Fig. 2 represents a kind of reflective substrate 21 that has by the formed coating 26 of the anti-UV coating composition of the present invention.As shown in Figure 2, because organic filler 25 has different specific refractory poweres with resin 22, so when the light from light source 23 enters by the formed coating 26 of the anti-UV coating composition of the present invention, because organic filler 25 is different with resin 22 specific refractory poweres, light repeatedly reflects in coating 26 inside, make the travel path of light prolong, easilier contact with inorganic particles 24, thus the ultraviolet effect of raising absorption.
Organic filler in the anti-UV coating composition of the present invention, its specific refractory power must be different with the specific refractory power of resin, and this organic filler is selected from by methacrylate resin, silicone resin and composition thereof, is preferably silicone resin.If the particle diameter of above-mentioned organic filler is too big, and light easily directly penetrates, and its UV assimilation effect is not good.The contriver discovers that the particle diameter of organic filler is preferably 0.1 micron to 10 microns, is preferably 1 micron to 5 microns, and the best is 1.8 microns to 2.4 microns.
The specific refractory power of the resin that the anti-UV coating composition of the present invention is comprised is at least 1.47, adds the specific refractory power that inorganic particles can improve resin, the highest specific refractory power to 2.0 that improves resin.The specific refractory power of the organic filler that the anti-UV coating composition of the present invention is comprised is 1.40 to 1.60.The anti-UV coating composition of the present invention comprises at least a specific refractory power organic filler different with resin, and the absolute value of the refringence of this organic filler and resin is at least about 0.07, is about 0.6 at the most.
Organic filler content in the anti-UV coating composition of the present invention is 1～500Wt% with respect to the amount of resin, is preferably 10～300Wt%, and the best is 30～200Wt%.Organic filler with respect to the amount of resin if be lower than 1Wt%, because of organic filler quantity very little, the light refraction poor effect can't effectively prolong optical path; But if be higher than 500Wt%, organic filler is difficult for being fixed on substrate surface, is easy to generate to come off.
Anti-UV coating composition of the present invention can comprise as required is familiar with this operator's known additives, includes but not limited to: stiffening agent (curing agent), flow agent (leveling agent), defoamer (defoamer), wetting agent (wetting agent) or static inhibitor (Anti-staticagent) or the like.The stiffening agent that the anti-UV coating composition of the present invention optionally adds, its effect are and resin produces chemical bond between molecule and the molecule, form interlinkage (Crosslinking).Stiffening agent used in the present invention is a personage institute well known of haveing the knack of this technology, such as: polymeric polyisocyanate (Polyisocyanate).
The anti-UV coating composition of the present invention can be coated any suitable substrates surface, for example optical element, glass, metal, alloy, computer housing, cement, woodenware, plastics, leather or stone material etc., especially optical element, the surface forms an anti-UV layer after the coating, plays to absorb ultraviolet effect.
The present invention also provides a kind of uvioresistant film, and it comprises an optical element, and at least one mask of this base material has at least one deck by the formed anti-UV layer of anti-UV coating composition of the present invention.
If the employed optical element of this uvioresistant film is with function distinguishing, including but not limited to: reflective substrate and transparent substrate are preferably reflective substrate.The kind of above-mentioned optical element is a plastic basis material, there is no particular restriction for this plastic basis material, can be any the technical field of the invention has and knows the known person of the knowledgeable usually, such as but not limited to: vibrin (polyesterresin), as polyethylene terephthalate (polyethylene terephthalate, PET) or Polyethylene Naphthalate (polyethylene naphthalate, PEN); Polyacrylate resin (polyacrylate resin), as polymethylmethacrylate (polymethyl methacrylate, PMMA); Polyimide resin (polyimide resin); Polyolefin resin (polyolefin resin) is as polyethylene (PE) or polypropylene (PP); Poly-cyclic olefin resins (polycycloolefin resin); Polycarbonate resin (polycarbonate resin); Polyurethane resin (polyurethaneresin); Cellulosetri-acetate (triacetate cellulose, TAC); Or the mixture of these materials.Wherein preferred: polyethylene terephthalate, polymethylmethacrylate, poly-cyclic olefin resins, cellulosetri-acetate or its mixture are more preferred from polyethylene terephthalate.The thickness of base material depends on the demand of the optical articles of wishing to get usually, and is preferable between about 16 microns (μ m) are to about 1000 microns.
Base material of the present invention can be reflective substrate.Above-mentioned reflective substrate can be the single or multiple lift structure, and wherein one or more layers can optionally be selected expanded plastic for use or contain the plastics of particle or be the two combination.By expanded plastic or contain the plastics of particle, can make base material have reflectivity properties.Above-mentioned particle comprises organic filler and inorganic particulate, and wherein the kind of inorganic particulate is to be familiar with this operator to know, for example: zinc oxide, silicon-dioxide, titanium dioxide, aluminum oxide, calcium sulfate, barium sulfate, lime carbonate or its mixture; The kind of organic filler also is to be familiar with this operator to know, for example: methacrylic resin, amido formate resin, silicone resin or its mixture.The diameter of above-mentioned particle or bubble is preferably 0.1 μ m to 5 μ m approximately between 0.01 μ m to 10 μ m.
Can use one or more commercially available diaphragms to constitute reflective substrate of the present invention.Can be used for commercially available diaphragm of the present invention such as but not limited to: produced by Teijin-Dopont company, commodity are by name
Or
The person; Produced by SKC company, commodity are by name
Produced by Toray company, commodity are by name
Or
The person; Produced by Mitsui company, commodity are by name
Or
The person; Produced by Tsujiden company, commodity are by name
The person; And by the production of Yupo company, commodity are by name
Or
Person etc.
Fig. 3 to Fig. 6 has described the concrete enforcement aspect that can be used for reflective substrate of the present invention.
Fig. 3 is a kind of preferable enforcement aspect that can be used for reflective substrate of the present invention, and wherein base material 410 is the three-layer plastic base materials that constituted by 41,42 and 44, and middle layer 42 contains inorganic particulate 43.The kind of base material such as this paper previous definition.For example, the three-layer plastic base material can be the PET resin, and for example commodity are by name
Commercially available diaphragm, series of strata comprise barium sulfate as inorganic particulate in the middle of this diaphragm-operated.
Fig. 4 is the another kind of preferable enforcement aspect that can be used for reflective substrate of the present invention, and wherein base material 510 is the three-layer plastic base materials that constituted by 51,52 and 54, and middle layer 52 is for having the expanded plastic of bubble 53.The kind of base material such as this paper previous definition.For example, the three-layer plastic base material can be the PET resin, and for example commodity are by name
Commercially available diaphragm, this diaphragm-operated middle layer has bubble.
Fig. 5 is another the preferable enforcement aspect that can be used for reflective substrate of the present invention, and wherein base material 610 is the three-layer plastic base materials that constituted by 61,62 and 64, and 62 inside, middle layer are contained inorganic particulate 63 and bubble 65 simultaneously.The kind of base material such as this paper previous definition.For example, the three-layer plastic base material can be the PP resin, and for example commodity are by name
Commercially available diaphragm, this diaphragm-operated middle layer still comprises titanium dioxide and lime carbonate as inorganic particulate except that having bubble.
Fig. 6 is another the preferable enforcement aspect that can be used for reflective substrate of the present invention, wherein base material 710 serve as reasons the layer 71 and 73 two plastic substrates that is constituted, it 71 includes more inorganic particulate 72 at the middle and upper levels, lower floor 73 contains less inorganic particulate 74.The kind of base material such as this paper previous definition.For example, two plastic substrates can be PET resin, PEN resin or its combination.Specific examples such as commodity are by name
Commercially available diaphragm, this diaphragm system is made of PET resin and PEN resin, and comprises barium sulfate as inorganic particulate.
Base material of the present invention also can be transparent substrate, and its structure can be single or multiple lift.The commercially available diaphragm that can be used for transparent substrate of the present invention includes but not limited to: produced by Toray company, commodity are by name
The person; By Mitsubishi production, commodity are by name
Or
The person; Produced by Toyobo company, commodity are by name
The person; And by the production of company of Japanese Supreme Being people-Du Pont (TDFJ), commodity are by name
Or
Person etc.
The thickness of the anti-UV layer of film of the present invention should be preferably 1 micron to 15 microns between 0.1 micron to 20 microns.
The anti-UV layer of film of the present invention can for example, utilize into rolling (roll to roll) continuous production technology according to the known any way manufacturing of the personage who is familiar with this skill, via the method manufacturing that comprises following steps:
(I) with components such as resin, inorganic particles, organic filler, solvents, optionally mix, form an anti-UV coating composition with known additive;
(II) should coat the optical element surface by anti-UV coating composition, to form a coating;
(III) heating of the optical element after will applying is 1 to several minutes, evaporating solvent, and carry out the thermofixation polyreaction.
If need, can repeat above steps, to obtain the anti-UV layer of plural layer.In addition, also can optionally further another surface of optical element also be coated with single or plural anti-UV layer.
Base material in the above-mentioned steps (II) can optionally be done the surface with corona (corona) or electricity slurry (plasma) and handle, to increase the adherence of its anti-UV coating composition.In addition, the coating process of anti-UV coating composition system is familiar with this operator and knows, for example: slit coating (slit Diecoating), nick version printing coating (micro gravure coating), roller coating (rollercoating) etc.Above-mentioned coating process can one or more be used in combination.
Usually, light source in the backlight module of indicating meter, as CCFL (CCFL), outer electrode fluorescent tube (EEFL), HCFL (HCFL), plane xenon light source or ultraviolet LED etc., its light of launching contains the UV-light of 300nm to 399nm and the visible light of 400nm to 780nm, and wherein the UV-light with 313nm is bigger to the injury of film material again.
According to a specific examples of the present invention, when optical element was reflective substrate, according to the ASTM903-96 standard method, the reflectivity that records film when wavelength 313nm was lower than 10%.And when optical element is transparent substrate, according to ASTM 903-96 standard method, the penetration coefficient that records film when wavelength 313nm also is lower than 10%, and this explanation can effectively be absorbed the ultraviolet ray of 313nm wavelength by the formed anti-UV layer of the anti-UV coating composition of the present invention.
According to a specific examples of the present invention, film of the present invention is according to ASTM G154 atmospheric exposure test standard method and ASTM E313 detection method, and the yellowness index changing value that records (Δ YI) is less than 2, so can effectively reduce the etiolation of film itself.
In addition, according to a specific examples of the present invention, when optical element was reflective substrate, film of the present invention can provide the reflectivity that reaches more than 97% in visible light wave zone 400～780nm scope, can effectively improve the briliancy of backlight module.
The film that the present invention has anti-UV layer can be applicable to the on glass of buildings in general (as exterior wall) or public transportation vehicle (as automobile), so that good anti-UV effect to be provided.The film that the present invention has anti-UV layer also can be applicable in the light source device, for example: advertising lamp box and flat-panel screens etc., especially can be used in the backlight liquid crystal display module, as reflectance coating, lampshade reflectance coating, diffusion barrier, diffuser plate or condensing film etc., so that the improvement effect to be provided.
Above-mentioned backlight module generally is divided into side type and straight-down negative, the light source device system of above-mentioned advertising lamp box as shown in Figure 7, light source device 800 comprises housing 84, inside casing 85 and diaphragm group 80, and wherein fluorescent tube 86 is positioned at the inside of inside casing 85, and diaphragm group 80 comprises diffusion barrier 81, light guiding plate 82 and reflectance coating 83.Fig. 8 is a direct type backlight module 220, comprises reflectance coating 221, fluorescent tube 222, diffuser plate 223, diffusion barrier 224, condensing film 225 and goes up diffusion barrier 226; Fig. 9 is a side type backlight module 230, comprises reflectance coating 231, fluorescent tube 232, light guiding plate 233, diffusion barrier 234, condensing film 235, goes up diffusion barrier 236 and lampshade reflectance coating 237.
Film of the present invention can strengthen briliancy, has good weathering resistance, and has the ultraviolet effect of absorption, and can effectively solve the phenomenon of base material yellow, reduces the aberration problem of LCD, reaches the purpose that strengthens the liquid-crystal display effect.
Below be the specific embodiment of technical solution of the present invention, this only is an exemplary applications, can not be interpreted as the restriction to claim protection domain of the present invention.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop within protection scope of the present invention.
One, the anti-UV coating composition of preparation
1, the anti-UV coating composition A of preparation
[Eterac 7363 with 92 gram methylacrylic acid resins (specific refractory power is 1.49), Eternal company] (solids component about 50%), add each 27.5 gram of solvent methylethylketone/toluene, under high-speed stirring (rotating speed 500rpm), add 2 gram 35nm titanium dioxide (specific refractory power is 2.72)/37 grams, 2 μ m silicone resin particle (specific refractory power is 1.42) (Tospearl 120E in regular turn, GE-Toshiba company), [Desmodur 3390 for 9.2 gram stiffening agents, Bayer company] (solids component about 75%), form 250 gram coating composition A (solids component about 40%).
2, anti-UV coating composition B
[Etertac 7363 with 64.0 gram methacrylic resins (specific refractory power is 1.49), Eternal company] (solids component about 50%), add each 36.3 gram of solvent methylethylketone/toluene, under high-speed stirring (rotating speed 500rpm), add 1.4 gram 35nm titanium dioxide (specific refractory power is 2.72)/69 grams, 2 μ m silicone resin particle (specific refractory power is 1.42) (Tospearl 120E in regular turn, GE-Toshiba company), [Desmodur 3390 for 6 gram stiffening agents, Bayer company] (solids component about 75%), form 250.0 gram coating composition B (solids component about 43%).
3, anti-UV coating composition C
[Etertac 7363 with 158.8 gram methacrylic resins (specific refractory power is 1.49), Eternal company] (solids component about 50%), add each 72.7 gram of solvent methylethylketone/toluene, under high-speed stirring (rotating speed 500rpm), add in regular turn 3.6 the gram 35nm titanium dioxide (specific refractory power is 2.72), 14.9 the gram stiffening agents [Desmodur 3390, Bayer company] (solids component about 75%), form 250.0 gram coating composition C (solids component about 43%).
4, anti-UV coating composition D
[Etertec 7363 with 64.0 gram acrylic resins (specific refractory power is 1.49), Eternal company] (solids component about 50%), add solvent methylethylketone, each 54.8 gram of toluene, under high-speed stirring (rotating speed 500rpm), add 1.4 gram 35nm zinc oxide (specific refractory power is 2.37)/69 grams, 2 μ m silicone resin micropartical (Tospearl 120E in regular turn, GE-Toshiba company), stiffening agent [desmodur3390, Bayer company] (solids component about 75%) 6 grams, form 250.0 gram coating composition D (solids component about 43%).
Inorganic particulate is a titanium dioxide among anti-UV coating composition A, B, the C, the difference of wherein anti-UV coating composition A and anti-UV coating composition B is the content of silicone resin particle, anti-UV coating composition C does not then contain the silicone resin micropartical, and the inorganic particulate among the anti-UV coating composition D then is a zinc oxide.Ratio by identical coating dry film thickness and identical inorganic particulate/resin can compare the influence that silicone resin particle content number is caused for anti-UV characteristic.
Two, preparation uvioresistant film of the present invention
To resist UV coating composition A to coat reflector plate with RDS paint daubs #16
On (thickness 150 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film adds up to the about 160 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement " QUV (UVB-313nm) irradiation 500 hours ", and do weather resistance test.
To resist UV coating composition A to coat reflector plate with RDS paint daubs #16
On (thickness 188 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film added up to the about 198 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
Embodiment 3
To resist UV coating composition A to coat reflector plate with RDS paint daubs #16
On (thickness 225 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film added up to the about 235 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
Embodiment 4
To resist UV coating composition B to coat reflector plate with RDS paint daubs #16
On (thickness 150 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film added up to the about 160 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
Embodiment 5
To resist UV coating composition B to coat reflector plate with RDS paint daubs #16
On (thickness 188 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film added up to the about 198 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
Embodiment 6
To resist UV coating composition B to coat reflector plate with RDS paint daubs #16
On (thickness 225 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film added up to the about 235 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
Embodiment 7
To resist UV coating composition C to coat reflector plate with RDS paint daubs #16
On (thickness 188 μ m, Teijin-Dupont company) base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film added up to the about 198 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
The coating that anti-UV coating D is disposed is coated reflector plate UX-188 (thickness 188 μ m with RDS paint daubs #16 with coating, Teijin-Dupont company) on the base material, with 100 ℃ of dryings one minute, can about 10 μ m after the drying film, add up to the about 198 μ m of total film thickness, leave standstill treated its maturation in seven days after, carry out optical characteristic measurement, and do weather resistance test.
Three, commercially available reflectance coating contrast
Comparative example 1
With thickness is the commercially available reflectance coating of 150 μ m
(Teijin-Dupont company) carries out optical characteristic measurement, and does weather resistance test.
Comparative example 2
With thickness is the commercially available reflectance coating of 188 μ m
(Teijin-Dupont company) carries out optical characteristic measurement, and does weather resistance test.
Comparative example 3
With thickness is the commercially available reflectance coating of 225 μ m
(Teijin-Dupont company) carries out optical characteristic measurement, and does weather resistance test.
Comparative example 4
With thickness is the commercially available reflectance coating of 225 μ m
(Teijin-Dupont company) carries out optical characteristic measurement, and does weather resistance test.
Comparative example 5
With thickness is the commercially available reflectance coating of 250 μ m
(Toray company) carries out optical characteristic measurement, and does weather resistance test.
Comparative example 6
With thickness is the commercially available reflectance coating of 250 μ m
(Toray company) carries out optical characteristic measurement, and does weather resistance test.
Four, testing method
Thickness test: utilize film thickness gauge PIM-100[TESA company], press down the thickness that testing sample is measured in the way of contact with 1N.
Reflectance test: utilize UV-light visible spectrometry Lamda 650[Perkin Elmer company], with the reflectivity of integrating sphere type ASTM 903-96 method measurement testing sample 200nm to 800nm wavelength, test gained result is as shown in the following Table I.
Utilize QUV weather resistance test machine [Q-Panel company], set with ASTM G154 method respectively, setting UVB 313nm fluorescent tube energy is 0.8W/m
2/ nm, envrionment conditions: under 60 ℃, sample is tested.Take out the reflectivity of diaphragm respectively at each time point (the 0th, 100,300 and 500 hour), shown in the test following tabulation three of gained result and Figure 10 to 23 with aforesaid method measurement testing sample.
Glossiness test: utilize glossmeter VG2000[Nippon Denshoku company], with the ASTMD523 method light source is projected to the testing sample surface with 60 ° of input angles, again in 60 ° of its surface glosses of reflection angle position measurement.Test gained result as shown in the following Table I.
Colourity test: utilize colourimeter Color Quest XE[Hunter Lab company], measure testing sample L, a, b, YI value according to standard and ASTM E313 method that CIE1976 formulates, test gained result is as shown in the following Table I.
Anti-UV xanthochromia test: utilize QUV weather resistance test machine [Q-Panel company], setting UVB313nm fluorescent tube energy is 0.8W/m
2/ nm, under 60 ℃, setting UVB 313nm fluorescent tube energy with ASTM G154 method respectively is 0.8W/m
2/ nm shone testing sample 100,300,500 hours in regular turn, took out sample size subsequently and measured yellowness index (YellowIndex) YI numerical value with ASTM E313 method, and calculate yellowness index changing value (Δ YI), the following tabulation two of test gained result.
Five, test result
Via above-mentioned reflectivity, glossiness, and the colourity testing method record embodiment 1-8 and each diaphragm-operated optical property of comparative example 1-6, and be recorded in table one.
Table one: each diaphragm-operated optical property
| Project | Glossiness (60 °) | Reflectivity (313nm, %) | Reflectivity (550nm, %) | L | a | | YI |
| Embodiment | |||||||
| 1 | 36.2 | 5.8 | 97.74 | 98.17 | -0.15 | 0.13 | 0.06 |
| |
33.0 | 5.5 | 98.20 | 98.36 | -0.20 | 0.33 | 0.41 |
| Embodiment 3 | 34.9 | 5.7 | 98.45 | 98.83 | -0.17 | 0.37 | 0.50 |
| Embodiment 4 | 2.6 | 5.5 | 97.35 | 98.04 | -0.17 | 0.27 | 0.32 |
| Embodiment 5 | 2.6 | 5.6 | 97.90 | 98.29 | -0.20 | 0.41 | 0.55 |
| Embodiment 6 | 2.6 | 5.5 | 98.19 | 98.37 | -0.22 | 0.58 | 0.85 |
| Embodiment 7 | 96 | 5.9 | 97.25 | 98.26 | -0.16 | 0.24 | 0.26 |
| |
2.6 | 4.4 | 97.60 | 98.32 | -0.23 | 0.32 | 0.37 |
| Comparative example 1 | 45.0 | 29.2 | 96.51 | 98.04 | -0.05 | -0.19 | -0.47 |
| Comparative example 2 | 45.3 | 28.6 | 97.13 | 98.12 | -0.04 | 0.03 | -0.05 |
| Comparative example 3 | 44.7 | 25.8 | 97.62 | 98.39 | -0.08 | 0.08 | 0.02 |
| Comparative example 4 | 20.0 | 64.0 | 97.65 | 98.26 | 0.32 | -0.63 | -1.01 |
| Comparative example 5 | 29.0 | 46.5 | 96.74 | 99.39 | 2.14 | -11.50 | -19.94 |
| Comparative example 6 | 26.0 | 5.9 | 96.73 | 98.59 | 0.35 | -4.16 | -7.63 |
By the result of table one as can be known---
1, the influence of glossiness: with the embodiment 1,2,3 of anti-UV coating A coating, its silicone resin micropartical and resin ratio are less, the surface is comparatively smooth, but incident light enters coating and via part particle refraction, reflection, so glossiness is respectively 36.2,33.0,34.9.Embodiment 4,5,6,8 with anti-UV coating B, D coating, its silicone resin micropartical is 200% of a resin, surface irregularity makes incident light enter coating and repeatedly reflects the reflected light that forms a lambert (Lambertian) diffusion through organic filler that glossiness is all 2.6.And embodiment 7 does not contain any silicone resin micropartical, so the surface is quite smooth smooth, and its glossiness is very high, the direct incident of light, reflection, and the glossiness measured value is 96.0.
2, the influence of reflectivity: embodiment 1,2,3 and 4,5,6 visible wavelength 550nm reflectivity are respectively 97.74%, 98.20%, 98.45% and 97.35%, 97.90%, 98.19%, show that the total film thickness increase can make visible wavelength 550nm reflectivity promote.Compare with the visible wavelength 550nm reflectivity of comparative example 1,2,3 with embodiment 1,2,3, all promoted about 1%, show that anti-UV coating A can promote the reflectivity of former reflective substrate.Result by embodiment 4,5,6 also demonstrates the effect that anti-UV coating B can make reflectivity promote in addition.The ultraviolet wavelength 313nm reflectivity of embodiment 1～7 than the ultraviolet wavelength 313nm reflectivity of comparative example 1～5, shows that anti-UV coating A, B, C have anti-ultraviolet function all less than 10%.And the inorganic particles that anti-UV coating D uses is a nano zine oxide, and the ultraviolet wavelength 313nm reflectivity of embodiment 8 possesses anti-ultraviolet function equally also less than 10%.
3. the influence of colourity: embodiment 1～8 compares and no significant difference with L, a, b, the YI data of comparative example 1,2,3, shows that anti-UV coating A, B, C, D can not influence the colourity performance of former reflective substrate.
Record embodiment 1-8 and each diaphragm of comparative example 1-6 in the yellow index variation value of each time point via above-mentioned anti-UV xanthochromia testing method, and be recorded in table two.In addition, above-mentioned diaphragm in the reflectivity of each time point system as Figure 10～shown in Figure 23.
Table two: QUV (UVB-313nm) irradiation yellow index variation
| | Shine | 100 hours | Shine | 300 hours | Shine | 500 hours Δ |
| Embodiment | ||||||
| 1 | 0.63 | 0.66 | 0.80 | |||
| |
0.50 | 0.52 | 0.69 |
| | Shine | 100 hours | Shine | 300 hours | Shine | 500 hours Δ YI |
| Embodiment 3 | 0.52 | 0.58 | 0.65 | |||
| Embodiment 4 | 0.46 | 0.50 | 0.56 | |||
| Embodiment 5 | 0.25 | 0.28 | 0.30 | |||
| Embodiment 6 | 0.38 | 0.44 | 0.47 | |||
| Embodiment 7 | 0.86 | 1.30 | 1.96 | |||
| |
0.82 | 1.22 | 1.86 | |||
| Comparative example 1 | 6.70 | 11.1 | 13.98 | |||
| Comparative example 2 | 5.59 | 11.17 | 14.02 | |||
| Comparative example 3 | 7.34 | 12.60 | 15.79 | |||
| Comparative example 4 | 5.67 | 6.53 | 7.53 | |||
| Comparative example 5 | 19.87 | 25.97 | 29.65 | |||
| Comparative example 6 | 0.13 | 1.74 | 2.48 |
By the result of table two and Fig. 8～Figure 21 as can be known---
1, embodiment 1～8 shone 100,300,500 hours with QUV with comparative example 1～6, and its yellowness index all elongates with irradiation time and increases gradually.Wherein, use embodiment 2, embodiment 5, the embodiment 7 of anti-UV coating A, B, C coating gained, after 500 hours, the yellowness index changing value is respectively 0.69,0.30,1.96, with the variation minimum of embodiment 5 with the QUV irradiation.The result shows: under identical coating dried film thickness and reflective substrate, the atomic addition of silicone resin increases, after can causing UV-light to enter coating layer, via repeatedly refraction between micropartical and the resin, make UV-light arrive the path propagation of base material, the number of times of contact inorganic particles increases, thereby has further promoted anti-UV.
2, embodiment 1～7 is through 0,100,300,500 hour reflection spectrum of QUV irradiation, and Figure 10 to Figure 16 finds that its visible wavelength 400～800nm zone has no significant change, the provable ability of using inorganic particles titanium dioxide to absorb UV-light.And use anti-UV coating D to be coated with the embodiment 8 of gained, and after 500 hours, the yellowness index changing value is 1.86 with the QUV irradiation, and this coating uses zinc oxide, and its anti-uv-ray is the same, so yellowness index changing value Δ YI is less than 2.0.
3, comparative example 1～5 can obviously be observed the yellowness index changing value all greater than more than 7.0 in QUV irradiation after 500 hours, and comparative example 6 is a commercial anti UV reflectance coating, and its yellowness index changing value is about 2.48, also is higher than embodiment 1～8.Further through QUV irradiation 0,100,300,500 as a child by comparative example 1～5, can find out reflectivity considerable change and the decline of visible wavelength 400～780nm, especially (400～550nm) declines change bigger blue light territory reflectivity, cause the numerical value of yellowness index to increase.
According to the reflectance test method, test implementation example 1～8 and comparative example 1～6 each diaphragm are in QUV weather resistance test machine [Q-Panel company], and setting UVB313nm, fluorescent tube energy are 0.8W/m
2The the 0th and 500 hour reflectivity under 60 ℃ of/the nm, envrionment conditions is recorded in table three.
500 hours reflectance varies of table three: QUV (UVB-313nm) irradiation relatively
By the result of table three as can be known---
1, the visible wavelength 450nm (blue light) of embodiment 1～6,8,550nm (green glow), 650nm (ruddiness) reflectivity shine 500 hours its reflectance varies values all less than 2.0% through QUV (UVB-313nm); demonstration inorganic particles titanium dioxide, zinc oxide can be protected former reflective substrate effectively with ultraviolet absorption.And along with the atomic ratio of organic filler silicone resin increases, can make UV-light enter coating layer after repeatedly reflect the path propagation that arrives base material, the number of times of contact inorganic particles increases, and lowers the injury of UV-light to base material, so reflectivity roughly can be kept and 0 hour numerical value.Though embodiment 7 comprises inorganic particles, yet, resinous principle does not contain the silicone resin micropartical, UV-light enters directly incident and reflection after the coating, contact inorganic particles number of times is few, ultraviolet ray can't effectively absorb, and then has influenced diaphragm character, make its in the reflectance varies value at visible wavelength 450nm, 550nm, 650nm place greater than the obtained reflectance varies of embodiment 1-6 diaphragm.
2, comparative example 1～5 is through QUV (UVB-313nm) irradiation 500 hours, and it all greater than more than 10%, shows that the blue region reflectivity descends in the reflectance varies rate of visible wavelength 450nm, and the base material yellowness index is also significantly promoted.In addition, the visible wavelength 450nm reflectance varies 2.7% of comparative example 6, than embodiment 1～8 2.0% with allowance below nominal size.
Above result shows, anti-UV coating composition of the present invention has quite superior character, no matter coat after the reflective substrate, be that the performance of colourity, the yellowness index of testing 500 hours through QUV (UVB-313nm) change or reflectance varies, all is better than other commercially available product.
Claims (26)
1. anti-ultraviolet paint composition, comprise inorganic particles and resin, it is characterized in that: also contain organic filler in the middle of this coating composition, described organic filler is selected from the group that is made of methacrylic resin, silicone resin and composition thereof, and its particle diameter is 0.1 micron to 10 microns; And described organic filler is different with the specific refractory power of resin, and the absolute value of the difference of both specific refractory poweres is at least 0.07, is at most 0.6.
2. anti-ultraviolet paint composition according to claim 1 is characterized in that: the specific refractory power of described organic filler is 1.40 to 1.60.
3. anti-ultraviolet paint composition according to claim 1 is characterized in that: the particle diameter of described organic filler is 1 micron to 5 microns.
4. anti-ultraviolet paint composition according to claim 1 is characterized in that: the quality of described organic filler is 1% to 500% of a resin quality.
5. anti-ultraviolet paint composition according to claim 4 is characterized in that: the quality of described organic filler is 10% to 300% of a resin quality.
6. anti-ultraviolet paint composition according to claim 1 is characterized in that: described organic filler is a silicone resin.
7. anti-ultraviolet paint composition according to claim 1 is characterized in that: described inorganic particulate is selected from the group that is made of zinc oxide, silicon-dioxide, titanium dioxide, zirconium white, aluminum oxide, barium sulfate, lime carbonate and composition thereof.
8. anti-ultraviolet paint composition according to claim 7 is characterized in that: described inorganic particulate is selected from the group that is made of zinc oxide, titanium dioxide and composition thereof.
9. anti-ultraviolet paint composition according to claim 1 is characterized in that: the particle diameter of described inorganic particulate is 1～1000 nanometer.
10. anti-ultraviolet paint composition according to claim 1 is characterized in that: the quality of described inorganic particulate is 0.1% to 100% of a resin quality.
11. anti-ultraviolet paint composition according to claim 1 is characterized in that: described resin is selected from the group that is made of acrylic resin, methacrylic resin, polyamide resin, Resins, epoxy, fluoroplast, polyimide resin, polyurethane resin, Synolac, vibrin and composition thereof.
12. anti-ultraviolet paint composition according to claim 11 is characterized in that: described resin is methacrylic resin or fluoroplast.
13. a uvioresistant film comprises an optical element, it is characterized in that: the uvioresistant coating that at least one mask of described optical element has one deck at least to be formed by the described coating composition of claim 1.
14. uvioresistant film according to claim 13 is characterized in that: described optical element is reflective substrate or transparent substrate.
15. uvioresistant film according to claim 14 is characterized in that: described optical element is the reflective substrate of single or multiple lift structure, records its yellowness index changing value (Δ YI) less than 2 according to ASTM G154 and ASTM E313 standard method.
16. uvioresistant film according to claim 15 is characterized in that: described reflective substrate is an expanded plastic, or contains the plastics of particle, or expanded plastic and contain the composition of particle plastics.
17. uvioresistant film according to claim 16 is characterized in that: described reflective substrate contains bubble and particle simultaneously.
18. uvioresistant film according to claim 17 is characterized in that: the diameter of described bubble and particle is 0.01 micron to 10 microns.
19. according to claim 16 or 17 or 18 described uvioresistant films, it is characterized in that: described particle is organic filler or inorganic particulate.
20. uvioresistant film according to claim 19 is characterized in that: described particle is an organic filler, and described organic filler is selected from the group that is made of methacrylic resin, amido formate resin, silicone resin and composition thereof.
21. uvioresistant film according to claim 19, it is characterized in that: described particle is an inorganic particulate, and described inorganic particulate is selected from the group that is made of zinc oxide, silicon-dioxide, titanium dioxide, aluminum oxide, calcium sulfate, barium sulfate, lime carbonate and composition thereof.
22. uvioresistant film according to claim 13 is characterized in that: the thickness of described optical element is 16 microns to 1000 microns.
23. uvioresistant film according to claim 13 is characterized in that: the thickness of described uvioresistant coating is 1 micron to 20 microns.
24. uvioresistant film according to claim 23 is characterized in that: the thickness of described uvioresistant coating is 3 microns to 15 microns.
25. uvioresistant film according to claim 13 is characterized in that: according to the ASTM903-96 standard method, the reflectivity that records this uvioresistant film when wavelength 313nm is lower than 10%, and it is arranged in the display backlight module and is used as reflectance coating.
26. uvioresistant film according to claim 13 is characterized in that: according to the ASTM903-96 standard method, the penetration coefficient that records this uvioresistant film when wavelength 313nm is lower than 10%, and it is arranged in the display backlight module and is used as diffusion barrier.
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| CN110698191B (en) * | 2019-10-28 | 2021-01-05 | 南京航空航天大学 | Biological ceramic material with ultraviolet high reflection |
| CN111169137B (en) * | 2019-12-31 | 2022-03-04 | 东莞市尼的科技股份有限公司 | Anti-ultraviolet protective film and preparation method thereof |
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