CN103214888A - Coating liquid for preparation of weather resistant optical grade hard coating film and corresponding hard coating film - Google Patents
Coating liquid for preparation of weather resistant optical grade hard coating film and corresponding hard coating film Download PDFInfo
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- CN103214888A CN103214888A CN2013100974682A CN201310097468A CN103214888A CN 103214888 A CN103214888 A CN 103214888A CN 2013100974682 A CN2013100974682 A CN 2013100974682A CN 201310097468 A CN201310097468 A CN 201310097468A CN 103214888 A CN103214888 A CN 103214888A
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Abstract
The present invention provides a coating liquid for preparation of a weather resistant optical grade hard coating film. The coating liquid includes the following components by weight: A. 30%-80% of an acrylate compound; B. 10%-40% of a reactive polymer containing 1%-20% of hydroxy or amino; C. 0.1%-10% of a photoinitiator; D. 0.5%-1% of a coupling agent; and E. 5%-20% of inorganic nanoparticles of 2-30 nm. In the present invention, after the coupling agent is added to the hard coating film coating liquid, lubricating property between inorganic nanoparticles is increased, agglomeration of the inorganic nanoparticles is decreased, the compatibility between the nanoparticles and an organic hardened layer is increased, and the weatherability of the hard coating film is improved. The present invention also provides a corresponding weather resistant optical grade hard coating film.
Description
Technical field
The present invention relates to a kind of coating fluid that is used to prepare weathering resistance optical grade cured film, relate in particular to a kind of cured film coating fluid of introducing behind the coupling agent; The present invention relates to corresponding weathering resistance optical grade cured film simultaneously, relates in particular to a kind of optical grade cured film with high rigidity, high transmission rate and lasting weathering resistance; The invention still further relates to the preparation method of above-mentioned coating fluid and cured film.
Background technology
In recent years, along with the application of transparent hardened film is more and more wider, technical requirements improves constantly, and the demand of cured film constantly rises.For example: (1) touch-screen cured film (ITO conducting film cured film); (2) demonstration field: liquid crystal display, mobile phone, MP4, notebook computer screen protection film, touch screen protective film; (3) in-mold decoration IMD field as various household electrical appliances panels, notebook computer shell, thin film switch etc., all applies to transparent hardened film in a large number, and this cured film has certain degree of hardness and crocking resistance, can play a very good protection.
Chinese invention patent application 201010566198.1 provides a kind of cured film that the plane shows that can be used in, it has added a spot of inorganic particulate in the middle of the cured film coating fluid, after ultraviolet ray (UV) is solidified, formation has the good acid-proof alkaline and the hardening coat of high rigidity, but can observe from sem test, and particle is at the skewness of organic film, exist tangible interfacial separation phenomenon between inorganic particulate and the organic film, the cohesiveness that causes hardening between rete and the base material reduces, make weathering resistance, problem such as warpage properties and heat-shrinkable is outstanding, increase the mist degree of cured film, reduced the transmittance of rete.Its reason is owing to there is the problem of consistency between inorganic rigid particle and the polymeric matrix.
Therefore, how to provide a kind of method that improves the consistency between inorganic particulate and the organic sclerosis rete to become the problem that industry need solve.
Summary of the invention
At the shortcoming of prior art, one of purpose of the present invention provides a kind of coating fluid of preparing weathering resistance optical grade cured film and preparation method thereof that is used to, and another object of the present invention provides a kind of weathering resistance optical grade cured film and preparation method thereof.
To achieve these goals, on the one hand, the invention provides a kind of coating fluid that is used to prepare weathering resistance optical grade cured film, by weight, it comprises following component:
The acrylic ester compound of A, 30%-80%,
The reactive polymer that contains 1%-20% hydroxyl or amino of B, 10%-40%;
The light trigger of C, 0.1%-10%;
D, 0.5%-1% coupling agent;
The inorganic nano-particle of the 2nm-30nm of E, 5%-20%.
Among the present invention, acrylic ester compound can be, dimethacrylate-1 for example, 4-butanediol ester, 1, ammediol dimethacrylate, propylene glycol diacrylate, two season penta triol acrylate, 2-ethyl pentaerythritol triacrylate, dihydroxymethyl butane pentaerythritol triacrylate.It should be noted that, in the material that step (1) is prepared, have the acrylic ester compound that two kinds, three kinds even four kinds of components all belong to 1-2 reactive functional group degree, have the acrylic ester compound that two kinds, three kinds even four kinds of components all belong to 3-5 reactive functional group degree.
Among the present invention, hydroxyl or amino reactive polymer can be, for example glycine triacrylate class, glycine esters of acrylic acid, epoxy acrylate class, urethane acrylate class, amino acrylates class or epoxy resin class.
Among the present invention; light trigger can be; for example 2; 4; 6;-trimethylbenzoyl diphenyl phosphine oxide (TPO), 2,2 ,-dimethoxy-2-phenyl methyl phenyl ketone (BDMK), 2-isopropyl thioxanthone (ITX), 2-hydroxymethyl phenyl-propane-1-ketone, benzoin dimethylether, 1-hydroxycyclohexylphenylketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone.
Used coupling agent can increase the cohesiveness between inorganic particulate and the organic polymer among the present invention.Because having, nano inoganic particle strengthens toughness reinforcing effect in superpolymer, be widely used in fields such as rubber, plastics, tackiness agent, coating, wherein nano inoganic particle is example with the nano silicon, when nano silicon contacts with wet air, " reaction " takes place in lip-deep Siliciumatom and water molecules, to keep the tetrahedral coordination of oxygen, satisfy the valency of Siliciumatom, water molecules can be irreversible or reversibly absorption is in its surface.Nano silicon has bigger specific surface area, existence with surface hydroxyl, has high reactive behavior, make nano-silicon dioxide particle that agglomeration take place easily, therefore need carry out surface modification treatment at it, purpose is to improve the physico-chemical property of nano silicon, improve its dispersed in polymkeric substance and with consistency, the mechanical property of polymkeric substance and weathering resistance are improved.The principle of adding coupling agent is that molecule one end of coupling agent is an alkyl, with the organic polymer molecular chain certain consistency is arranged, and the other end is a polar group, with inorganic particulate certain chemical action is arranged, and can increase the consistency in inorganic nano-particle and the organic polymer.
Coupling agent among the present invention can be, for example silane coupling agent, titanate coupling agent, maleic anhydride inoculated polypropylene acid resin.
Among the present invention, add coupling agent in the cured film coating fluid after, the lubricity between the inorganic nano-particle increases, and has reduced the agglomeration between the inorganic nano-particle, consistency between nanoparticle and the organic hardened layer increases, and has improved the weathering resistance of cured film.
Another embodiment according to the present invention, acrylic ester compound is selected from following one or more: dimethacrylate-1,4-butanediol ester, 1, ammediol dimethacrylate, propylene glycol diacrylate, two season penta triol acrylate, 2-ethyl pentaerythritol triacrylate, dihydroxymethyl butane pentaerythritol triacrylate
Another embodiment according to the present invention, hydroxyl or amino reactive polymer are selected from following one or more: glycine triacrylate class, glycine esters of acrylic acid, epoxy acrylate class, urethane acrylate class, amino acrylates class or epoxy resin class.
Another embodiment according to the present invention; light trigger is selected from following one or more: 2; 4; 6;-trimethylbenzoyl diphenyl phosphine oxide (TPO), 2; 2 ,-dimethoxy-2-phenyl methyl phenyl ketone (BDMK), 2-isopropyl thioxanthone (ITX), 2-hydroxymethyl phenyl-propane-1-ketone, benzoin dimethylether, 1-hydroxycyclohexylphenylketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone.
Another embodiment according to the present invention, coupling agent are selected from following one or more: silane coupling agent, titanate coupling agent, maleic anhydride inoculated polypropylene acid resin; The inorganic nano-particle of 2nm～30nm is a kind of in nanometer grade silica, titanium dioxide, the lime carbonate.
Another embodiment according to the present invention, silane coupling agent are γ-An Bingjisanyiyangjiguiwan KH550, γ-(2.3-epoxy third oxygen) propyl trimethoxy silicane KH560, γ-(methacryloxypropyl) propyl trimethoxy silicane KH570, vinyltriethoxysilane A-151 or vinyltrimethoxy silane A-171.
On the other hand, the invention provides the method for the above-mentioned coating fluid of preparation, it comprises the steps:
(1) by weight, prepare following material:
The acrylic ester compound of A, 30%-80%,
The reactive polymer that contains 1%-20% hydroxyl or amino of B, 10%-40%;
The light trigger of C, 0.1%-10%;
D, 0.5%-1% coupling agent;
The inorganic nano-particle of the 2nm-30nm of E, 5%-20%;
(2) room temperature and do not have UV-light and sun-exposed condition under, step (1) is prepared various components in the material joins in the mixing vessel and fully stir;
(3) mixture that obtains after step (2) mixing is filtered with removal of contamination, obtain the cured film coating fluid.
Another aspect the invention provides a kind of novel weathering resistant optical grade cured film, and it comprises:
Base material film, and
Be coated on the hardened layer that solidifies back formation on the base material film with above-mentioned coating fluid.
Further, base material film is PET or TAC film.
It is pointed out that cured film provided by the present invention is mainly used in the plane and shows.
On the one hand, the invention provides a kind of method for preparing above-mentioned optical grade cured film again, it comprises the steps:
I, aforesaid coating fluid is coated on the base material film;
II, with UV-irradiation, make coating fluid on base material film, solidify and form hardened layer.
Wherein, in the steps A, the coating process of coating fluid is a line rod coating method, a kind of in the coating method that flows, dip coated method or the spraying coating method.Among the step B, be preferably with microwave-excitation type electrodeless ultraviolet lamp and shine, irradiation energy is 300-700mj/cm
2
Compared with prior art, the present invention possesses following beneficial effect:
Among the present invention, behind the interpolation coupling agent, the lubricity between the inorganic nano-particle increases, and has reduced the agglomeration between the inorganic nano-particle in the cured film coating fluid.Because an end of modifier molecules is an alkyl, with the organic polymer molecular chain certain consistency is arranged, the other end is a polar group, with mineral filler certain chemical action is arranged, the adding of coupling agent improves dispersiveness and the consistency of inorganic particulate in cured film, after UV-light (UV) is solidified, reduce the mist degree and the percent thermal shrinkage of cured film, improved transmittance, hardness and the weathering resistance of cured film.
Description of drawings
Fig. 1 is among the embodiment 1, the coating design sketch of cured film;
Fig. 2 is among the embodiment 1, the manufacturing flow chart of cured film.
Embodiment
Embodiment 1
One, the preparation of cured film coating fluid:
(1) prepare following material:
(2) in room temperature, not have UV-light and sun exposure, relative air humidity be under about 60% the condition, step (1) is prepared various components in the material joins in the mixing vessel and fully stirred 15 minutes;
(3) mixture that obtains after step (2) mixing is filtered with removal of contamination, obtain the cured film coating fluid.
Two, the preparation of optics cured film:
As shown in Figure 1, with line rod coating method the cured film coating fluid of above preparation is coated on the base material film (for example thickness 188 microns the PET of Du Pont film).As shown in Figure 2, after drying treatment, be 300mj/cm with microwave-excitation type electrodeless ultraviolet lamp, irradiation energy
2Irradiation makes the cured film coating fluid solidify to form hardened layer on base material, and then obtains cured film (base material+coating fluid solidifies the hardened layer that the back forms).Survey its performance and see Table 1.
Embodiment 2
One, the preparation of cured film coating fluid:
(1) prepare following material:
(2) in room temperature, not have UV-light and sun exposure, relative air humidity be under about 60% the condition, step (1) is prepared various components in the material joins in the mixing vessel and fully stirred 15 minutes;
(3) mixture that obtains after step (2) mixing is filtered with removal of contamination, obtain the cured film coating fluid.
Two, the preparation of optics cured film:
As shown in Figure 1, with line rod coating method the cured film coating fluid of above preparation is coated on the base material film (for example thickness 188 microns the PET of Du Pont film).As shown in Figure 2, after drying treatment, be 500mj/cm with microwave-excitation type electrodeless ultraviolet lamp, irradiation energy
2Irradiation makes the cured film coating fluid solidify to form hardened layer on base material, and then obtains cured film (base material+coating fluid solidifies the hardened layer that the back forms).Survey its performance and see Table 1.
Embodiment 3
One, the preparation of cured film coating fluid:
(1) prepare following material:
(2) in room temperature, not have UV-light and sun exposure, relative air humidity be under about 60% the condition, step (1) is prepared various components in the material joins in the mixing vessel and fully stirred 15 minutes;
(3) mixture that obtains after step (2) mixing is filtered with removal of contamination, obtain the cured film coating fluid.
Two, the preparation of optics cured film:
As shown in Figure 1, with line rod coating method the cured film coating fluid of above preparation is coated on the base material film (for example thickness 188 microns the PET of Du Pont film).As shown in Figure 2, after drying treatment, be 700mj/cm with microwave-excitation type electrodeless ultraviolet lamp, irradiation energy
2Irradiation is solidified the cured film coating fluid and is formed hardened layer on base material, and then obtains cured film (base material+coating fluid solidifies the hardened layer of formation afterwards).Survey its performance and see Table 1.
Table 1
After embodiment 1-3 process thermotolerance and the winter hardiness test, find the mist degree no change of cured film, illustrate that weathering resistance improves
Observe through sem test, find out that the phase interface between inorganic particulate and the organic sclerosis rete is fuzzy, consistency increases, and by the test of angularity and percent thermal shrinkage, the cohesiveness that draws cured film and base material obviously improves.
Attached: the dependence test method of weighing the preparation characteristic of cured film:
1, hardness test
Draw test with BY type pencil hardness meter (750g) and advanced drawing pen (6B-6H), according to drawing to hard order, demarcate the hardness of cured film coating with the maximum hardness pencil label that does not produce cut, with reference to the GB/T6739-2006 standard by soft.
2, coating adhesion test (coat fastness)
Hundred lattice methods: draw the little lattice of 100 2mm * 2mm in coat side 20mm * 20mm square area, in little lattice surface, peel off with 180 angles again after 90 seconds, observe little lattice and glued situation about falling with the adhesive tape sticking of 3M.Specifically with reference to U.S. ASTM D3359 standard.
3, percent thermal shrinkage
Print to be measured is cut into the specification of 15cm * 15cm,, sample is placed on the sheet glass in the baking oven with 150 ℃ of heating 30min and 60min, treat the sample cooling dimensional change of length between measuring mark afterwards with the length of the about 120mm of marking pen mark.Be applicable to the GB/T12027-2004 standard.
4, transmittance/mist degree
Adopt WGT-S transmittance/mist degree determinator to measure, with reference to U.S. ASTM D1003 standard.
5, resistance to acids and bases
After using 10% hydrochloric acid soaking at room temperature 24h and 5% yellow soda ash soaking at room temperature 24h respectively, check every Hardenability, specifically with reference to the GB/T1763-1979 standard.
6, heating crimp tendency (angularity)
To be cut into the sample of 182cm * 257cm specification, and add hard formation (HC) the open and flat baking oven of putting into that makes progress, timing 60min slowly is cooled to room temperature then when room temperature is warming up to 150 ℃, takes out print.With the height of four angle warpages of height calipers measurement print, with the angularity numerical value of greatest measure as this print.
7, Steel Wool wearability
With No. 0000 Steel Wool, with 100g/cm
2Or 200/cm
2The reactive force that waits does not rub back and forth in the surface of hardening coat, observes the situation of coatingsurface cut, indicates with the maximum friction number of times that cut do not occur, with reference to the GB/T1768-2006 standard.
8, thermotolerance
Under 150 ℃ temperature, every performance that tested sample is placed check cured film behind the 30min is with reference to the GB/T1735-79 standard.
9, winter hardiness
Under-20 ℃ temperature, every performance that tested sample is placed check cured film behind the 168h is with reference to the GB/T1763-1979 standard.
Though the present invention discloses in conjunction with the preferred embodiments, these embodiment are not in order to limit scope of the invention process.Any those of ordinary skill in the art in not breaking away from invention scope of the present invention, when can doing suitable improvement, promptly everyly anyly according to the present invention did is equal to replacement, all in protection scope of the present invention.
Claims (10)
1. coating fluid that is used to prepare weathering resistance optical grade cured film, by weight, it comprises following component:
The acrylic ester compound of A, 30%-80%;
The reactive polymer that contains 1%-20% hydroxyl or amino of B, 10%-40%;
The light trigger of C, 0.1%-10%;
The coupling agent of D, 0.5%-1%;
The inorganic nano-particle of the 2nm-30nm of E, 5%-20%.
2. coating fluid as claimed in claim 1, wherein, described acrylic ester compound is selected from following one or more: dimethacrylate-1,4-butanediol ester, 1, ammediol dimethacrylate, propylene glycol diacrylate, two season penta triol acrylate, 2-ethyl pentaerythritol triacrylate, dihydroxymethyl butane pentaerythritol triacrylate.
3. coating fluid as claimed in claim 1, wherein, described hydroxyl or amino reactive polymer are selected from following one or more: glycine triacrylate class, glycine esters of acrylic acid, epoxy acrylate class, urethane acrylate class, amino acrylates class or epoxy resin class.
4. coating fluid as claimed in claim 1; wherein; described light trigger is selected from following one or more: 2; 4; 6;-trimethylbenzoyl diphenyl phosphine oxide (TPO), 2,2 ,-dimethoxy-2-phenyl methyl phenyl ketone (BDMK), 2-isopropyl thioxanthone (ITX), 2-hydroxymethyl phenyl-propane-1-ketone, benzoin dimethylether, 1-hydroxycyclohexylphenylketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone.
5. coating fluid as claimed in claim 1, wherein, described coupling agent is selected from following one or more: silane coupling agent, titanate coupling agent, maleic anhydride inoculated polypropylene acid resin; The inorganic nano-particle of described 2nm～30nm is a kind of in nanometer grade silica, titanium dioxide, the lime carbonate.
6. coating fluid as claimed in claim 5, wherein, described silane coupling agent is γ-An Bingjisanyiyangjiguiwan KH550, γ-(2.3-epoxy third oxygen) propyl trimethoxy silicane KH560, γ-(methacryloxypropyl) propyl trimethoxy silicane KH570, vinyltriethoxysilane A-151 or vinyltrimethoxy silane A-171.
7. method for preparing one of claim 1-6 described coating fluid, it comprises the steps:
(1) by weight, prepare following material:
The acrylic ester compound of A, 30%-80%,
The reactive polymer that contains 1%-20% hydroxyl or amino of B, 10%-40%;
The light trigger of C, 0.1%-10%;
D, 0.5%-1% coupling agent;
The inorganic nano-particle of the 2nm-30nm of E, 5%-20%;
(2) room temperature and do not have UV-light and sun-exposed condition under, step (1) is prepared various components in the material joins in the mixing vessel and fully stir;
(3) mixture that obtains after step (2) mixing is filtered with removal of contamination, obtain the cured film coating fluid.
8. novel weathering resistant optical grade cured film, it comprises:
Base material film, and
Be coated on the hardened layer that solidifies back formation on the described base material film with the described coating fluid of one of claim 1-6.
9. cured film as claimed in claim 8, wherein, described base material film is PET or TAC film.
10. method for preparing the described optical grade cured film of one of claim 8-9, it comprises the steps:
I, the described coating fluid of one of claim 1-6 is coated on the base material film;
II, with UV-irradiation, make described coating fluid on described base material film, solidify and form hardened layer.
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Application publication date: 20130724 |