CN104031525A - Coating liquid with high refractive index for transparent holographic film and preparation method thereof - Google Patents
Coating liquid with high refractive index for transparent holographic film and preparation method thereof Download PDFInfo
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- CN104031525A CN104031525A CN201410243300.2A CN201410243300A CN104031525A CN 104031525 A CN104031525 A CN 104031525A CN 201410243300 A CN201410243300 A CN 201410243300A CN 104031525 A CN104031525 A CN 104031525A
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Abstract
The invention discloses a coating liquid with high refractive index for a transparent holographic film and a preparation method thereof. The coating liquid with high refractive index comprises a nanomaterial precursor, butanone, ethanediamine and epoxy resin E-40, wherein the nanomaterial precursor comprises butanone, an acetic acid zinc salt, sodium sulfide and methyl butyl cellulose. The preparation method of the coating liquid with the high refractive index is that the nanomaterial is subjected to in-situ synthesis in the precursor of organic resin or resin, and the prepared coating liquid has the characteristics of high refractive index and high light transmittance.
Description
Technical field
The present invention relates to a kind of high refractive index coating liquid and preparation method thereof, particularly relate to a kind of high refractive index coating liquid for transparent holographic film and preparation method thereof, belong to laser antifalsification technology field.
Background technology
At present, conventional optical holography film is generally made up of functional coatings such as plastic basic unit, separating layer, information layer, medium layer, seal glue-lines.In preparation process, first separating layer is coated on plastic basic unit, then in separating layer, be coated with information layer, again the plastics film that scribbles separating layer and information layer is carried out to mold pressing on moulding press, hologram pattern is impressed on information layer, and on the information layer that is printed on hologram pattern, plate medium layer, or coat again offset printing layer, thus prepare can display holography pattern optical holography film.Above-mentioned plastic basic unit is generally PET, BOPP, PE, PVC thermoplastic material, separating layer be generally there is release, the polyolefin resin of moulding property and tackiness, print the resin that glue-line mostly is a class and has thermoset, tackiness, information layer is the carrier of accepting holographic information, holographic information is by certain tension force, pressure, temperature, the processing such as cooling, by the precise grating mold pressing on embossment to information layer, precise grating is made up of the complicated convex-concave striped of 800-1500 bar/mm, and therefore the voltage-dependent characteristic to information layer and rebound resilience have high requirement.Along with the progress of the research to holographic image carrier material and transparent holographic optics, information layer material is also constantly updated, but be mainly macromolecular material, such as acrylic resin, urethane resin, polyphenylene resin and aminoresin etc., the transparency and the specific refractory power that focus on improving organic information layer material of research.
The premiere feature of medium layer is the precise grating of protection information layer, can be transparent inorganic layer, opaque metal layer or semiconductor layer.Because the specific refractory power of most organic materialss only 1.4 ~ 1.5, need to could improve specific refractory power by chemistry or physical method modification, at present, introducing optical function group is the effective ways of raising organic materials specific refractory power, but the method is difficult for realizing industrialization.And the specific refractory power of inorganic materials is greater than organic polymer material conventionally, therefore coating inorganic material medium layer can improve the diffracted intensity of holographic optics film.The preparation technology of medium layer adopts plated film mode substantially at present, mainly taking metallic aluminium as medium layer material, can obtain beautiful in colour, lifelike hologram image.And for transparent holographic film, must select transparent material as zinc sulphide, titanium dioxide is medium layer, could obtain transparent hologram pattern, but, transparent inorganic medium layer of the prior art is subject to the impact of high temperature deposition technique larger, homogeneity is difficult to control, cause the poor transparency of coating, and, the existence of transparent medium coating, just there is information layer/medium layer (the first interface), two interfaces of medium layer/seal glue-line (second contact surface), may cause being disturbed by the diffraction pattern at second interface at the diffraction pattern at first interface, thereby make the technical indicator such as diffraction efficiency and signal to noise ratio of transparent optical holographic film lower than the holographic film of aluminizing.
In view of this, the inventor studies this, develops specially a kind of high refractive index coating liquid for transparent holographic film and preparation method thereof, and this case produces thus.
Summary of the invention
The object of this invention is to provide a kind of coating liquid for transparent holographic film and preparation method thereof, described preparation method is the presoma situ nano materials at organic resin or resin, and the coating liquid making has the feature of high refractive index and high transmission rate.
To achieve these goals, solution of the present invention is:
A kind of high refractive index coating liquid for transparent holographic film, comprise nano material presoma, butanone, quadrol and epoxy resin E-40, wherein, described nano material presoma comprises butanone, Zinc diacetate dihydrate, nine hydrated sodium sulfides and methyl butyl Mierocrystalline cellulose, wherein
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 0-15%) proportioning is as follows:
Butanone (water ratio 1%) 40-72
Epoxy resin E-40 16
Quadrol 0-8
Precursor solution 0-45.
For a high refractive index coating liquid preparation method for transparent holographic film, comprise the steps:
Step 1, the preparation of nano material presoma: make solvent with butanone, taking methyl butyl Mierocrystalline cellulose as anti-settling agent, take in proportion Zinc diacetate dihydrate and nine hydrated sodium sulfides, join in butanone, utilize 6-8KW power ultrasonic, set the frequency of 80-100KHz, at 20-30 DEG C of temperature, shake 2-5min and make uniform dispersion system;
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
In its reaction process, main chemical equation is as follows:
2H
2oZnSO
4+ 9H
2oNa
2s → ZnS precipitation+Na
2sO
4+ 11H
2o
Step 2, high refractive index coating liquid synthesize: make solvent with butanone (water ratio 1%), taking epoxy resin E-40 as main film forming substance, add a certain amount of linking agent quadrol, and introduce the nano material presoma that step 1 makes, under 20-30 DEG C of room temperature normal pressure, with the speed stirring reaction 1.5-3h of 500-700 rev/min, make the coating liquid of high refractive index;
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 0-15%) proportioning is as follows:
Butanone (water ratio 1%) 40-72
Epoxy resin E-40 16
Quadrol 0-8
Precursor solution 0-45.
Above-mentioned high refractive index coating liquid preparation method is the presoma situ nano materials at organic resin or resin, also has high transmission rate when the coating liquid making has high refractive index.Described high refractive index coating liquid can directly be coated on thermoplastic organic polymer film, then solidifies continuously through the soft pressure of grating and low temperature, directly forms transparent holographic film.High refractive index coating liquid of the present invention is fully used for reference organic materials and inorganic materials in specific refractory power, transmittance, the advantage separately of the aspect such as thermoplasticity and non-deformability, the nano inorganic media particle with high refractive index is incorporated into the information layer of organic material, thereby obtain having concurrently the hybrid compound coating homogeneous system of information layer and medium layer function, reach the maximized while in specific refractory power, also can obtain high transparency, the application of above-mentioned high refractive index coating liquid not only can be avoided structure and functional compatibility and the matching problem between original information layer and medium layer, reduce the coating number of plies of holographic film and the complicacy of light transmission, and reduce diffraction pattern and disturb, and overcome the technical barrier of high temperature deposition on information layer impact, process simplification.
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment
embodiment 1
A kind of high refractive index coating liquid for transparent holographic film, comprise nano material presoma, butanone, quadrol and epoxy resin E-40, wherein, described nano material presoma comprises butanone, Zinc diacetate dihydrate, nine hydrated sodium sulfides and methyl butyl Mierocrystalline cellulose, wherein
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 0-15%) proportioning is as follows:
Butanone (water ratio 1%) 70
Epoxy resin E-40 16
Quadrol 8
Precursor solution 6.
For a high refractive index coating liquid preparation method for transparent holographic film, comprise the steps:
Step 1, the preparation of nano material presoma: make solvent with butanone, taking methyl butyl Mierocrystalline cellulose as anti-settling agent, take in proportion Zinc diacetate dihydrate and nine hydrated sodium sulfides, join in butanone, utilize 6KW power ultrasonic, set the frequency of 80KHz, at 25 DEG C of temperature, shake 3 min and make uniform dispersion system;
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
In its reaction process, main chemical equation is as follows:
2H
2oZnSO
4+ 9H
2oNa
2s → ZnS precipitation+Na
2sO
4+ 11H
2o
Step 2, high refractive index coating liquid synthesize: make solvent with butanone (water ratio 1%), taking epoxy resin E-40 as main film forming substance, add a certain amount of linking agent quadrol, and introduce the nano material presoma that step 1 makes, under 25 DEG C of room temperature normal pressures, with the speed stirring reaction 2h of 500 revs/min, make high refractive index and obtain coating liquid
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 2%) proportioning is as follows:
Butanone (water ratio 1%) 70
Epoxy resin E-40 16
Quadrol 8
Precursor solution 6
Above-mentioned high refractive index coating liquid preparation method is the presoma situ nano materials at organic resin or resin, also has high transmission rate when the coating liquid making has high refractive index.
embodiment 2
A kind of high refractive index coating liquid for transparent holographic film, comprise nano material presoma, butanone, quadrol and epoxy resin E-40, wherein, described nano material presoma comprises butanone, Zinc diacetate dihydrate, nine hydrated sodium sulfides and methyl butyl Mierocrystalline cellulose, nano material presoma component and content described in the present embodiment are identical with embodiment 1, difference is only that each parts by volume ratio of nano material presoma, butanone, quadrol and epoxy resin E-40 is different, refers to following high refractive index coating liquid preparation method step 2.
For a high refractive index coating liquid preparation method for transparent holographic film, comprise the steps:
Step 1, the preparation of nano material presoma: make solvent with butanone, taking methyl butyl Mierocrystalline cellulose as anti-settling agent, take in proportion Zinc diacetate dihydrate and nine hydrated sodium sulfides, join in butanone, utilize 7KW power ultrasonic, set the frequency of 85KHz, at 20 DEG C of temperature, shake 2 min and make uniform dispersion system;
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
In its reaction process, main chemical equation is as follows:
2H
2oZnSO
4+ 9H
2oNa
2s → ZnS precipitation+Na
2sO
4+ 11H
2o
Step 2, high refractive index coating liquid synthesize: make solvent with butanone (water ratio 1%), taking epoxy resin E-40 as main film forming substance, add a certain amount of linking agent quadrol, and introduce the nano material presoma that step 1 makes, under 20 DEG C of room temperature normal pressures, with the speed stirring reaction 2.5h of 600 revs/min, make high refractive index and obtain coating liquid
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 5%) proportioning is as follows:
Butanone (water ratio 1%) 66
Epoxy resin E-40 16
Quadrol 3
Precursor solution 15
embodiment 3
A kind of high refractive index coating liquid for transparent holographic film, comprise nano material presoma, butanone, quadrol and epoxy resin E-40, wherein, described nano material presoma comprises butanone, Zinc diacetate dihydrate, nine hydrated sodium sulfides and methyl butyl Mierocrystalline cellulose, nano material presoma component and content described in the present embodiment are identical with embodiment 1, difference is only that each parts by volume ratio of nano material presoma, butanone, quadrol and epoxy resin E-40 is different, refers to following high refractive index coating liquid preparation method step 2.
For a high refractive index coating liquid preparation method for transparent holographic film, comprise the steps:
Step 1, the preparation of nano material presoma: make solvent with butanone, taking methyl butyl Mierocrystalline cellulose as anti-settling agent, take in proportion Zinc diacetate dihydrate and nine hydrated sodium sulfides, join in butanone, utilize 7KW power ultrasonic, set the frequency of 90KHz, at 30 DEG C of temperature, shake 5 min and make uniform dispersion system;
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
In its reaction process, main chemical equation is as follows:
2H
2oZnSO
4+ 9H
2oNa
2s → ZnS precipitation+Na
2sO
4+ 11H
2o
Step 2, high refractive index coating liquid synthesize: make solvent with butanone (water ratio 1%), taking epoxy resin E-40 as main film forming substance, add a certain amount of linking agent quadrol, and introduce the nano material presoma that step 1 makes, under 30 DEG C of room temperature normal pressures, with the speed stirring reaction 2.5h of 700 revs/min, make high refractive index and obtain coating liquid
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 10%) proportioning is as follows:
Butanone (water ratio 1%) 48
Epoxy resin E-40 16
Quadrol 6
Precursor solution 30
Above-mentioned high refractive index coating liquid preparation method is the presoma situ nano materials at organic resin or resin, also has high transmission rate when the coating liquid making has high refractive index.
embodiment 4
A kind of high refractive index coating liquid for transparent holographic film, comprise nano material presoma, butanone, quadrol and epoxy resin E-40, wherein, described nano material presoma comprises butanone, Zinc diacetate dihydrate, nine hydrated sodium sulfides and methyl butyl Mierocrystalline cellulose, nano material presoma component and content described in the present embodiment are identical with embodiment 1, difference is only that each parts by volume ratio of nano material presoma, butanone, quadrol and epoxy resin E-40 is different, refers to following high refractive index coating liquid preparation method step 2.
For a high refractive index coating liquid preparation method for transparent holographic film, comprise the steps:
Step 1, the preparation of nano material presoma: make solvent with butanone, taking methyl butyl Mierocrystalline cellulose as anti-settling agent, take in proportion Zinc diacetate dihydrate and nine hydrated sodium sulfides, join in butanone, utilize 7KW power ultrasonic, set the frequency of 100KHz, at 27 DEG C of temperature, shake 4 min and make uniform dispersion system;
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
In its reaction process, main chemical equation is as follows:
2H
2oZnSO
4+ 9H
2oNa
2s → ZnS precipitation+Na
2sO
4+ 11H
2o
Step 2, high refractive index coating liquid synthesize: make solvent with butanone (water ratio 1%), taking epoxy resin E-40 as main film forming substance, add a certain amount of linking agent quadrol, and introduce the nano material presoma that step 1 makes, under 27 DEG C of room temperature normal pressures, with the speed stirring reaction 3h of 700 revs/min, make high refractive index and obtain coating liquid
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 15%) proportioning is as follows:
Butanone (water ratio 1%) 40
Epoxy resin E-40 16
Quadrol 8
Precursor solution 45
Above-mentioned high refractive index coating liquid preparation method is the presoma situ nano materials at organic resin or resin, also has high transmission rate when the coating liquid making has high refractive index.
Table 1 is specific refractory power and the transmittance of the prepared high refractive index coating liquid of embodiment 1-4, and the amount by changing nano material presoma of finding is adjusted the volume fraction of nano-zinc sulfide, can change the specific refractory power of the specific refractory power of high refractive index coating liquid.
Table 1: specific refractory power and the transmittance of the prepared high refractive index coating liquid of embodiment 1-4
| ZnS volume fraction | 0% | 2% | 5% | 10% | 15% |
| High refractive index coating liquid specific refractory power | 1.45 | 1.47 | 1.50 | 1.55 | 1.60 |
| High refractive index coating liquid transmittance | 91% | 91% | 90% | 88% | 86% |
Specific refractory power theoretical value: epoxy resin specific refractory power 1.45, zinc sulphide specific refractory power 2.45
Can draw from embodiment 1 ~ 4 specific refractory power of high refractive index coating liquid and the testing data of transmittance, along with the increase of zinc sulphide volume fraction, specific refractory power also increases thereupon, but transmittance can decrease, when zinc sulphide volume fraction is during at 2%-15%, it also can obtain high transparency when specific refractory power reaches high value.
Above-described embodiment non-limiting product form of the present invention and style, suitable variation or modification that any person of an ordinary skill in the technical field does it, all should be considered as not departing from patent category of the present invention.
Claims (2)
1. the high refractive index coating liquid for transparent holographic film, it is characterized in that: comprise nano material presoma, butanone, quadrol and epoxy resin E-40, wherein, described nano material presoma comprises butanone, Zinc diacetate dihydrate, nine hydrated sodium sulfides and methyl butyl Mierocrystalline cellulose, wherein
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
High refractive index coating liquid component and content proportioning are as follows:
Butanone 40-72
Epoxy resin E-40 16
Quadrol 0-8
Precursor solution 0-45.
2. for a high refractive index coating liquid preparation method for transparent holographic film, it is characterized in that: comprise the steps:
Step 1, the preparation of nano material presoma: make solvent with butanone, taking methyl butyl Mierocrystalline cellulose as anti-settling agent, take in proportion Zinc diacetate dihydrate and nine hydrated sodium sulfides, join in butanone, utilize 6-8KW power ultrasonic, set the frequency of 80-100KHz, at 20-30 DEG C of temperature, shake 2-5min and make uniform dispersion system;
The each component of precursor solution and content (weight part) proportioning are as follows:
Zinc diacetate dihydrate 4.8
Nine hydrated sodium sulfides 4.4
Butanone 77
Methyl butyl Mierocrystalline cellulose 13.8
In its reaction process, main chemical equation is as follows:
2H
2oZnSO
4+ 9H
2oNa
2s → ZnS(precipitation)+Na
2sO
4+ 11H
2o;
Step 2, high refractive index coating liquid synthesize: make solvent with butanone (water ratio 1%), taking epoxy resin E-40 as main film forming substance, add a certain amount of linking agent quadrol, and introduce the nano material presoma that step 1 makes, under 20-30 DEG C of room temperature normal pressure, with the speed stirring reaction 1.5-3h of 500-700 rev/min, make the coating liquid of high refractive index;
High refractive index coating liquid component and content (parts by volume, corresponding zinc sulphide volume fraction is 0-15%) proportioning is as follows:
Butanone (water ratio 1%) 40-72
Epoxy resin E-40 16
Quadrol 0-8
Precursor solution 0-45.
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| CN201410243300.2A CN104031525B (en) | 2014-06-04 | 2014-06-04 | A kind of high index of refraction coating liquid for transparent holographic film and preparation method thereof |
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