CN104945647B - A kind of preparation method of anti-reflection PET film - Google Patents
A kind of preparation method of anti-reflection PET film Download PDFInfo
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- CN104945647B CN104945647B CN201510176148.5A CN201510176148A CN104945647B CN 104945647 B CN104945647 B CN 104945647B CN 201510176148 A CN201510176148 A CN 201510176148A CN 104945647 B CN104945647 B CN 104945647B
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Abstract
The invention belongs to organic film materials to be modified field, provides a kind of preparation method of anti-reflection PET film.By the organic inorganic hybridization of butyl methacrylate, styrene and acrylic acid cadmium, hydridization, branched materials are prepared, this material can generate micropore in curing molding in material system, surface index of refraction can be effectively reduced by being coated onto PET film surface.Macromolecular of the invention is branched, hybrid material, can form micropore, polymer material is attached to PET film surface by coating instrument (sol evenning machine), PET film light transmittance can be made to improve to 92% or so.
Description
Technical field
The invention belongs to organic film materials to be modified field, provides a kind of preparation method of anti-reflection PET film., pass through
On PET film surface, coated polymer material enables to meet the optics such as display so as to improve the antireflection performance of film
Translucent effect required by element.
Background technology
Polyethylene terephthalate (PET) film has good mechanical property, preferable gas (oxygen, dioxy
Change carbon and steam) barrier property, wider use temperature range (- 60-120 DEG C), excellent optical property and electrical insulation properties,
Its application field is related to packaging film, electronic apparatus insulating film, inflaming retarding membrane, copy film, drafting film, air-conditioning film, Electric radiant Heating Film, building dress
Decorations film etc..
Though China is flat-panel monitor big country at present, on some key materials such as optical polyester film, it is still necessary to be treated
Further development.The present invention is in polyester film surface coated polymer material to reaching antireflection purpose.To improve light
The optical property of the translucency, especially polyester film etc. of material is learned, needs to carry out antireflection modification to material surface.
In optical device, the thang-kng energy of reflection, the refraction, not only influence optical element of optical element surface；And
These reflected lights can also form stray light in instrument, influence the image quality of optical instrument.In order to solve these problems, usually
Certain thickness single-layer or multi-layer film i.e. optical anti-reflective film (or antireflective film) is plated on the surface of optical element, in order to subtract
The reflected light of small element surface increases the light transmittance of optical element.The use of anti-reflection film is to solve the problems, such as these effective means
One of.
Organic/inorganic hybridization material is a kind of finely dispersed heterogeneous material, organic phase and inorganic alternate interfacial area
Greatly, interaction is strong, make clearly interface thicken, wherein at least have at least one dimension of the size of a phase in nanometer number
The level of magnitude, even up to " molecule is compound ".Therefore, with single organic or inorganic polymer phase ratio, organic inorganic hybridization
Material has apparent performance advantage in optical transparence, tunable refractive index etc..
In addition, micropore can be also formed in organic/inorganic hybridization material forming process, the refraction of the air in these holes
Relatively low rate is 1.0, and light wave can pass through in these holes in addition, reduces diffusing reflection and further reduces effective refractive index, reaches
To the purpose for improving antireflection.
Invention content
It is an object of the invention to：A kind of preparation method of anti-reflection PET film is provided, is arranged after being handled using material surface
The mode of particle effectively raises the visible light transmittance rate of PET film, makes its light transmittance relatively low 88% before untreated
More than 90% present is increased, there is more apparent raising.
The technical solution adopted by the present invention to solve the technical problems is：A kind of preparation method of anti-reflection PET film, in fact
It is as follows to apply step：
(1) methyl methacrylate, styrene and acrylic acid cadmium are subjected to emulsion polymerization, obtain methyl methacrylate, benzene
The random copolymerization emulsion particle of ethylene and acrylic acid；
(2) the random copolymerization emulsion particle obtained in step (1) is diluted, and is spun on PET film surface, it is dry, it must increase
Saturating PET film.
Preferably, the light transmittance of the anti-reflection PET film is greater than or equal to 90%.
Preferably, the latex particle size range is between 30-45nm.
Preferably, specific implementation step is：
(1) methyl methacrylate, styrene, acrylic acid cadmium and initiator, emulsifier, solvent are added in reactor
Form reaction system；It is stirred to react at a temperature of nitrogen atmosphere, 60 DEG C -80 DEG C 4-6 hours, obtains methyl methacrylate, benzene
The random copolymerization emulsion particle lotion of ethylene and acrylic acid, is sealed.
(2) in a nitrogen environment, by the lotion obtained in step (1) with being diluted, using sol evenning machine by the dilute of gained
The good film of spin coating is placed in vacuum drying oven after drying and both obtains in pretreated PET film surface by the lotion applicator after releasing
Anti-reflection PET film.
Preferably, the methyl methacrylate is 1 with styrene mass ratio:1-1.5, the acrylic acid cadmium are methyl
Methyl acrylate and the 0.5-1.5% of styrene quality summation, the initiator content are methyl methacrylate in reaction system
The 1-2% of the quality summation of ester, styrene and acrylic acid cadmium；The emulsifier is methyl methacrylate, benzene in reaction system
The 2-4% of the quality summation of ethylene and acrylic acid cadmium；The solvent be deionized water, with system in methyl methacrylate,
Styrene and the ratio of acrylic acid cadmium quality summation are 3-5:1.
Preferably, in step (1), initiator used is potassium peroxydisulfate, and emulsifier used is dodecyl sodium sulfate.
Preferably, in step (2), extension rate is 10 times.
Preferably, in the step (1), specific charging sequence is：Water and emulsifier are firstly added, at 60 DEG C, is stirred
Mix 5min；Using constant pressure funnel, the 50% of monomer total amount is added in reaction system, and 30min is added dropwise to complete；It will be remaining
Monomer, acrylic acid cadmium, initiator mix, and 30min is added dropwise to complete under constant pressure, increase temperature, react several hours.
Preferably, PET film preprocess method is in the step (2)：By PET film successively by acetone, alcohol
Film is then placed on drying 12 hours in 70 DEG C of vacuum drying ovens, after the completion of dry, under oxygen atmosphere, uses plasma by washing
Body pre-processes 5min, W=400w.
Preferably, in the step (2), the sol evenning machine coating duration of runs is 20s, and preceding 5s rotating speeds are 450r/min, after
15s rotating speeds are 900r/min.
The beneficial effects of the invention are as follows：The preparation method of a kind of anti-reflection PET film provided by the invention, using common rotation
Diluting emulsion is spin-coated on pet sheet face by coating method, and the emulsion particle of acquisition is made to be evenly spaced in pet sheet face, the arrangement meeting of emulsion particle
Generate the micropore between particle, so as to decline surface refraction index, improve PET light transmittances, make its light transmittance from it is untreated it
Preceding relatively low 88% increases more than 90% present, there is more apparent raising.
Description of the drawings
The present invention is further described with reference to the accompanying drawings and examples.
Fig. 1 is PET infrared spectrums after spin coating, in 3000cm-1There is absorption peak in place, this is because styrene in styrene-acrylic emulsion
Caused, this illustrates that latex particle can be successfully fixed on pet sheet face by spin coating.
Fig. 2 be different acrylic acid cadmium contents emulsion particle diameter and 10 times dilution after light transmittance test.
Specific embodiment
In conjunction with the accompanying drawings, the present invention is further explained in detail.These attached drawings are simplified schematic diagram, only with
Illustration illustrates the basic structure of the present invention, therefore it only shows composition related to the present invention.
The preparation of PET film：
By the mylar sheet that about 100 sizes cut out are (3 × 3cm), number is washed with acetone, ethyl alcohol successively
It is secondary, polyester film is then put into 70 DEG C of vacuum drying 12h in vacuum drying oven, is taken out, it is pre- with plasma under oxygen atmosphere
5min, W=400w are handled, is sealed.
The light transmittance for testing PET film is 88%.
Embodiment 1
(1) preparation of hydridization, branched polymer material
Measure 60mL water, 10mL butyl methacrylates, 11mL styrene, 0.21g acrylic acid cadmium, 0.21g potassium peroxydisulfates
(using 10mL water dissolutions) and 0.8g dodecyl sodium sulfates；By 40mL water, 0.8g dodecyl sodium sulfates and 0.1g potassium peroxydisulfates
Three-necked flask is added in, stirs 5min；With constant pressure funnel by monomer 50% (i.e. 5mL butyl methacrylates and 6mL benzene second
Alkene) three-necked flask is instilled, about 30min is dripped off；Again by residual monomer, initiator and acrylic acid cadmium, instilled with constant pressure funnel
Flask, about 30min drip off, meanwhile, temperature is promoted to 60 DEG C using oil bath device, stirs lower sustained response 5h；Reaction is completed
After collect solution.
(2) preparation of anti-reflection PET film
Branched, the hybrid material deionized water that prepare are diluted 10 times, using sol evenning machine (during sol evenning machine coating operating
Between for 20s, 15s rotating speeds are 900r/min after preceding 5s rotating speeds are 450r/min) solution diluted is coated in it is processed
Film is dried 0.5h by the surface of PET film in 70 DEG C of vacuum drying oven later, and anti-reflection PET film is made.
Test methyl methacrylate, styrene and acrylic acid the average grain diameter of random copolymerization emulsion particle be：
34.36nm。
It tests its light transmittance and has been increased to 92.5% compared with 88% before coating.
Embodiment 2
(1) preparation of hydridization, branched polymer material
Measure 100mL water, 10mL butyl methacrylates, 10mL styrene, 0.1g acrylic acid cadmium, 0.20g potassium peroxydisulfates
(using 10mL water dissolutions) and 0.4g dodecyl sodium sulfates；By 40mL water, 0.4g dodecyl sodium sulfates and 0.1g potassium peroxydisulfates
Three-necked flask is added in, stirs 5min；With constant pressure funnel by monomer 50% (i.e. 5mL butyl methacrylates and 5mL benzene second
Alkene) three-necked flask is instilled, about 30min is dripped off；Again by residual monomer, initiator, flask is instilled with constant pressure funnel, about
30min is dripped off, meanwhile, temperature is promoted to 70 DEG C using oil bath device, stirs lower sustained response 3.5h；It is collected after the completion of reaction
Solution.
(2) preparation of anti-reflection PET film
Branched, the hybrid material deionized water that prepare are diluted 10 times, using sol evenning machine (during sol evenning machine coating operating
Between for 20s, 15s rotating speeds are 900r/min after preceding 5s rotating speeds are 450r/min) solution diluted is coated in it is processed
Film is dried 0.5h by the surface of PET film in 70 DEG C of vacuum drying oven later, and anti-reflection PET film is made.
Test methyl methacrylate, styrene and acrylic acid the average grain diameter of random copolymerization emulsion particle be：
32.12nm.
It tests its light transmittance and has been increased to 91.4% compared with 88% before coating.
Embodiment 3
(1) preparation of hydridization, branched polymer material
Measure 80mL water, 10mL butyl methacrylates, 15mL styrene, 0.375g acrylic acid cadmium, 0.5g potassium peroxydisulfates
(using 10mL water dissolutions) and 1g dodecyl sodium sulfates；40mL water, 1g dodecyl sodium sulfates and 0.25g potassium peroxydisulfates are added in
Three-necked flask stirs 5min；Monomer 50% (i.e. 5mL butyl methacrylates and 8mL styrene) is dripped with constant pressure funnel
Enter three-necked flask, about 30min is dripped off；Again by residual monomer, initiator, flask, about 30min drops are instilled with constant pressure funnel
It is complete, meanwhile, temperature is promoted to 80 DEG C using oil bath device, stirs lower sustained response 2.5h；Solution is collected after the completion of reaction.
(2) preparation of anti-reflection PET film
Branched, the hybrid material deionized water that prepare are diluted 10 times, using sol evenning machine (during sol evenning machine coating operating
Between for 20s, 15s rotating speeds are 900r/min after preceding 5s rotating speeds are 450r/min) solution diluted is coated in it is processed
Film is dried 0.5h by the surface of PET film in 70 DEG C of vacuum drying oven later, and anti-reflection PET film is made.
Test methyl methacrylate, styrene and acrylic acid the average grain diameter of random copolymerization emulsion particle be：
42.28nm.
It tests its light transmittance and has been increased to 91.2% compared with 88% before coating.
Embodiment 4
(1) preparation of hydridization, branched polymer material
Measure 80mL water, 10mL butyl methacrylates, 12mL styrene, 0.33g acrylic acid cadmium, 0.33g potassium peroxydisulfates
(using 10mL water dissolutions) and 0.66g dodecyl sodium sulfates；By 40mL water, 0.66g dodecyl sodium sulfates and 0.16g persulfuric acid
Potassium adds in three-necked flask, stirs 5min；With constant pressure funnel by monomer 50% (i.e. 5mL butyl methacrylates and 6mL benzene second
Alkene) three-necked flask is instilled, about 30min is dripped off；Again by residual monomer, initiator, flask is instilled with constant pressure funnel, about
30min is dripped off, meanwhile, temperature is promoted to 60 DEG C using oil bath device, stirs lower sustained response 5h；It is collected after the completion of reaction molten
Liquid.
(2) preparation of anti-reflection PET film
Branched, the hybrid material deionized water that prepare are diluted 10 times, using sol evenning machine (during sol evenning machine coating operating
Between for 20s, 15s rotating speeds are 900r/min after preceding 5s rotating speeds are 450r/min) solution diluted is coated in it is processed
Film is dried 0.5h by the surface of PET film in 70 DEG C of vacuum drying oven later, and anti-reflection PET film is made.
Test methyl methacrylate, styrene and acrylic acid the average grain diameter of random copolymerization emulsion particle be：
41.45nm.
It tests its light transmittance and has been increased to 91.4% compared with 88% before coating.
Comparative example 1
(1) preparation of hydridization, branched polymer material
80mL water, 10mL butyl methacrylates, 12mL styrene, 0g acrylic acid cadmium, 0.33g potassium peroxydisulfates is measured (to use
10mL water dissolutions) and 0.66g dodecyl sodium sulfates；By 40mL water, 0.66g dodecyl sodium sulfates and 0.16g potassium peroxydisulfates
Three-necked flask is added in, stirs 5min；With constant pressure funnel by monomer 50% (i.e. 5mL butyl methacrylates and 6mL benzene second
Alkene) three-necked flask is instilled, about 30min is dripped off；Again by residual monomer, initiator, flask is instilled with constant pressure funnel, about
30min is dripped off, meanwhile, temperature is promoted to 60 DEG C using oil bath device, stirs lower sustained response 5h；It is collected after the completion of reaction molten
Liquid.
(2) preparation of anti-reflection PET film
Branched, the hybrid material deionized water that prepare are diluted 10 times, using sol evenning machine (during sol evenning machine coating operating
Between for 20s, 15s rotating speeds are 900r/min after preceding 5s rotating speeds are 450r/min) solution diluted is coated in it is processed
Film is dried 0.5h by the surface of PET film in 70 DEG C of vacuum drying oven later, and anti-reflection PET film is made.
Test methyl methacrylate, styrene and acrylic acid the average grain diameter of random copolymerization emulsion particle be：
25.38nm.
What test its light transmittance compared with 88% before coating to become for 88.1%, without big variation.
Using above-mentioned desirable embodiment according to the present invention as enlightenment, by above-mentioned description, relevant staff is complete
Various changes and amendments can be carried out without departing from the scope of the technological thought of the present invention' entirely.The technology of this invention
Property range is not limited to the content on specification, it is necessary to determine its technical scope according to right.
Claims (10)
1. a kind of preparation method of anti-reflection PET film, implementation step are as follows：
(1) methyl methacrylate, styrene and acrylic acid cadmium are subjected to emulsion polymerization, obtain methyl methacrylate, styrene
With the random copolymerization emulsion particle of acrylic acid cadmium；
(2) the random copolymerization emulsion particle obtained in step (1) is diluted, and is spun on PET film surface, it is dry, obtain anti-reflection PET
Film.
2. a kind of preparation method of anti-reflection PET film as described in claim 1, it is characterised in that：The anti-reflection PET film
Light transmittance is greater than or equal to 90%.
3. a kind of preparation method of anti-reflection PET film as described in claim 1, it is characterised in that：The latex particle size model
It is trapped among between 30-45nm.
4. such as a kind of preparation method of anti-reflection PET film of claim 1-3 any one of them, it is characterised in that：Specific implementation
Step is：
(1) methyl methacrylate, styrene, acrylic acid cadmium and initiator, emulsifier, solvent are added in reactor and formed
Reaction system；It is stirred to react at a temperature of nitrogen atmosphere, 60 DEG C -80 DEG C 4-6 hours, obtains methyl methacrylate, styrene
With the random copolymerization emulsion particle lotion of acrylic acid cadmium, it is sealed；
(2) in a nitrogen environment, the lotion obtained in step (1) is diluted with deionized water, using sol evenning machine by gained
Dilution after lotion applicator in pretreated PET film surface, by the good film of spin coating be placed in vacuum drying oven it is dry after
Up to anti-reflection PET film.
5. a kind of preparation method of anti-reflection PET film as claimed in claim 4, it is characterised in that：
The methyl methacrylate is 1 with styrene mass ratio:1-1.5, the acrylic acid cadmium for methyl methacrylate with
The 0.5-1.5% of styrene quality summation, the initiator content are methyl methacrylate, styrene and third in reaction system
The 1-2% of the quality summation of olefin(e) acid cadmium；The emulsifier is methyl methacrylate, styrene and acrylic acid cadmium in reaction system
Quality summation 2-4%；The solvent is methyl methacrylate, styrene and acrylic acid in deionized water, with system
The ratio of cadmium quality summation is 3-5:1.
6. a kind of preparation method of anti-reflection PET film as claimed in claim 4, it is characterised in that：It is used to draw in step (1)
Hair agent is potassium peroxydisulfate, and emulsifier used is dodecyl sodium sulfate.
7. a kind of preparation method of anti-reflection PET film as described in right wants 4, it is characterised in that：In step (2), extension rate
It is 10 times.
8. a kind of preparation method of anti-reflection PET film as claimed in claim 4, it is characterised in that：In the step (1), tool
Body charging sequence is：Water and emulsifier are firstly added, at 60 DEG C, stirs 5min；Using constant pressure funnel, by monomer total amount
50% add in reaction system, and 30min is added dropwise to complete；Residual monomer, acrylic acid cadmium, initiator are mixed, under constant pressure
30min is added dropwise to complete, and is increased temperature, is reacted several hours, and the monomer is methyl methacrylate and styrene.
9. a kind of preparation method of anti-reflection PET film as claimed in claim 4, it is characterised in that：PET in the step (2)
Film preprocess method is：By PET film successively by acetone, ethanol wash, then film is placed in 70 DEG C of vacuum drying ovens
It is 12 hours dry, after the completion of dry, under oxygen atmosphere, 5min, W=400w are pre-processed with plasma.
10. a kind of preparation method of anti-reflection PET film as claimed in claim 4, it is characterised in that：It is even in the step (2)
The glue machine coating duration of runs is 20s, and preceding 5s rotating speeds are 450r/min, and rear 15s rotating speeds are 900r/min.
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| CN105753337B (en) * | 2016-03-02 | 2018-12-04 | 同济大学 | A kind of preparation method of environmentally protective inexpensive anti-reflection film |
| CN112143009A (en) * | 2020-09-19 | 2020-12-29 | 上海施恺新材料技术有限公司 | PET film with easily-separated surface |
| CN112679775A (en) * | 2020-12-18 | 2021-04-20 | 天津宝兴威科技股份有限公司 | Preparation method of anti-reflection PET film for liquid crystal writing board |
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