CN106405715B - A kind of preparation method and application of PVA film for polarizer - Google Patents
A kind of preparation method and application of PVA film for polarizer Download PDFInfo
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- CN106405715B CN106405715B CN201610988577.7A CN201610988577A CN106405715B CN 106405715 B CN106405715 B CN 106405715B CN 201610988577 A CN201610988577 A CN 201610988577A CN 106405715 B CN106405715 B CN 106405715B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002096 quantum dot Substances 0.000 claims abstract description 28
- 239000012153 distilled water Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 239000004014 plasticizer Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000004090 dissolution Methods 0.000 claims abstract description 6
- 239000012046 mixed solvent Substances 0.000 claims abstract description 6
- 238000004043 dyeing Methods 0.000 claims abstract description 5
- 239000003292 glue Substances 0.000 claims abstract description 5
- 238000012937 correction Methods 0.000 claims abstract description 4
- 230000001681 protective effect Effects 0.000 claims abstract description 4
- 230000008961 swelling Effects 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 229910017604 nitric acid Inorganic materials 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 235000011187 glycerol Nutrition 0.000 claims description 7
- 239000006228 supernatant Substances 0.000 claims description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000000975 dye Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 4
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 claims description 3
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052740 iodine Inorganic materials 0.000 claims description 3
- 239000011630 iodine Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 241001062009 Indigofera Species 0.000 abstract description 2
- 238000010030 laminating Methods 0.000 abstract 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- 239000010408 film Substances 0.000 description 39
- 239000004372 Polyvinyl alcohol Substances 0.000 description 36
- 229920002451 polyvinyl alcohol Polymers 0.000 description 36
- 239000004973 liquid crystal related substance Substances 0.000 description 8
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- ILJSQTXMGCGYMG-UHFFFAOYSA-N triacetic acid Chemical compound CC(=O)CC(=O)CC(O)=O ILJSQTXMGCGYMG-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 210000002858 crystal cell Anatomy 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003384 imaging method Methods 0.000 description 2
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 description 2
- 229940006461 iodide ion Drugs 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000012286 potassium permanganate Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 208000002177 Cataract Diseases 0.000 description 1
- 229920002284 Cellulose triacetate Polymers 0.000 description 1
- 208000010412 Glaucoma Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 208000003464 asthenopia Diseases 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- XTEGARKTQYYJKE-UHFFFAOYSA-N chloric acid Chemical compound OCl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-N 0.000 description 1
- 229940005991 chloric acid Drugs 0.000 description 1
- OSVXSBDYLRYLIG-UHFFFAOYSA-N chlorine dioxide Inorganic materials O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000019771 cognition Effects 0.000 description 1
- 210000000695 crystalline len Anatomy 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000004384 eye physiology Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
- 208000002780 macular degeneration Diseases 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000001525 retina Anatomy 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 230000010415 tropism Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
- G02B5/305—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks including organic materials, e.g. polymeric layers
Landscapes
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Carbon And Carbon Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
- Polarising Elements (AREA)
Abstract
The invention discloses a kind of preparation methods of PVA film for polaroid, it is to be uniformly blended into water-soluble graphene quantum dots after mixing PVA powder and plasticizer, it is subsequently poured into the in the mixed solvent of methanol and distilled water composition, mixed dissolution stirs 6~12h and forms mixed solution at 70 DEG C~90 DEG C, standing and defoaming simultaneously forms a film, and obtains polarized light property after carrying out washing swelling, dyeing, extension and correction.It is that the above-mentioned PVA film with doped graphene quantum dot is made with TAC film, protective film and pressure-sensitive glue laminating the invention also discloses a kind of polaroid, the addition of graphene quantum dot can effectively prevent " indigo plant leakage " phenomenon, and improve the humidity resistance of polaroid.
Description
Technical field
The present invention relates to polaroid fields, a kind of preparation method more particularly to PVA film for polaroid and its answer
With.
Background technique
As information interchange and transmitting increasingly increase severely, display device has become crowd as its main carrier and material base
The object of more scientist's research and probes, wherein liquid crystal display is the most widely used display device.Liquid crystal imaging must rely on
Light polarizing film, the mechanism of action are as follows: the polarizing film of two panels absorption axiss in vertical state is attached to liquid crystal cell two sides, when no applied voltage
When, light is unilateral without any display through polarizing.When the voltage for being applied to liquid crystal cell two sides causes the rotation of liquid crystal molecule, make to pass through
The direction of vibration of the polarised light of liquid crystal layer changes, and the light of charged image part is absorbed, and shows image or number, it is seen that
Polaroid is indispensable in liquid crystal imaging.
Current more common light polarizing film is iodine polarizing film, and dye series polarizing film is taken second place, and the light transmittance of light polarizing film and
Degree of polarization is already close to theoretical value, but the moisture-proof of light polarizing film, hot property are wait improve.
In addition, display device often there are problems that leaking blue light.The light of blue light i.e. 400~500nm wave band, blue light can penetrate
Crystalline lens reaches retina, and optical damage is caused to it, accelerates the oxidation of macular area cell, generates a large amount of free radicals, cause white
A possibility that cataract or glaucoma, macular area degenerates, induces human eye macular degeneration, can increase, visual fatigue is caused to rise, developing production to physiology of eye
It is raw to influence.As the problem of cognition of the people to health is more and more stronger, and blue light is leaked in display, is urgently to be resolved.
Summary of the invention
The present invention provides a kind of preparation method and applications of PVA film for polaroid, and which overcome the prior arts
Polaroid present in shortcoming.
The technical solution adopted by the present invention to solve the technical problems is: a kind of preparation side of the PVA film for polaroid
Method, comprising the following steps:
1) graphene quantum dot is prepared, the graphene quantum dot is water-soluble and diameter no more than 10nm；
2) it is uniformly blended into graphene quantum dot after taking PVA powder and plasticizer to mix, is subsequently poured into methanol and distilled water group
At in the mixed solvent, mixed dissolution stirs 6~12h and forms mixed solution at 70 DEG C~90 DEG C, and standing and defoaming simultaneously forms a film；Its
Middle PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 5~40g:0.5~10g:5~20ml:60~120ml,
And concentration of the graphene quantum dot in mixed solution is 0.1ppm~10ppm；
3) by the PVA film of formation carry out washing swelling, dyeing, extension and correction after obtain polarized light property, then prior to
30~90min is dried under 30 DEG C~50 DEG C of cryogenic temperature, dries 10~60min then at 60 DEG C~80 DEG C of high-temperature temperature sections.
Preferably, concentration of the graphene quantum dot in mixed solution is 1ppm~5ppm.
Preferably, the PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:5
~20ml:60~120ml.
Preferably, the plasticizer is glycerine, the PVA powder: glycerine: methanol: the mass volume ratio of distilled water
For 5~40g:1.5~5g:5~20ml:60~120ml.
Preferably, the PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:8
~12ml:60~120ml.
Preferably, in step 1), the preparation method of the graphene quantum dot is: the concentrated sulfuric acid and dense nitre is added in graphene
In acid, it is ultrasonically treated 5~15h, the acid that distilled water is diluted and is centrifuged in removal solution is then added, obtained solid is dissolved in
In the sodium hydroxide solution that pH is 10~13, moves into hydrothermal reaction kettle and react 10~14h at 180 DEG C~220 DEG C；Wherein graphite
Alkene: the concentrated sulfuric acid: the mass volume ratio of concentrated nitric acid is 20~30mg:3~8ml concentrated sulfuric acid: 10~20ml concentrated nitric acid.
Preferably, in step 1), the preparation method of the graphene quantum dot is: graphene oxide is dispersed in water,
Concentrated ammonia liquor mixing is added to move back into hydrothermal reaction kettle, in 280 DEG C~320 DEG C 6~10h of reaction, after being cooled to room temperature in separation
Layer clear liquid；Wherein the ratio of graphene oxide and concentrated ammonia liquor is 80~120mg:20~40ml.
Preferably, in step 1), the preparation method of the graphene quantum dot is: sulfuric acid and nitric acid being mixed and are placed on ice
In bath, graphene is added while stirring, sodium chlorate is slowly added to after 1~3h, adition process continues 30min~90min, to chloric acid
After being completely dissolved 40~60h is stirred at room temperature in mixed solution by sodium, is centrifuged the liquid of top 2/3rds after standing overnight
Obtain supernatant, adjustment supernatant pH value to 6~7 is then charged into bag filter and is placed in distilled water and is purified and removed big
Size piece is concentrated and is freeze-dried.
A kind of polaroid including above-mentioned PVA film, covers the TAC film in PVA film opposing sides, covers in one of them TAC
The pressure-sensing glue of the protective film of film opposite exterior lateral sides and another TAC film opposite exterior lateral sides.
Preferably, the polaroid is iodine polarizing piece or dyestuff polaroid, the PVA film with a thickness of 20~60 μm.
Compared to the prior art, the invention has the following advantages:
Graphene quantum dot of the invention has very strong quantum confined effect and edge effect, shows excellent photoelectricity
Characteristic, hypotoxicity, good biocompatibility and stability etc., by the way that graphene quantum dot is added in PVA film and is made partially
Mating plate can effectively improve its humidity resistance.In addition, graphene quantum dot can effectively absorb blue light, so can effectively prevent
" indigo plant leakage " phenomenon, can in polaroid field development and application values.
Invention is further described in detail with reference to the accompanying drawings and embodiments；But one kind of the invention is used for polaroid
The preparation method and applications of PVA film be not limited to the embodiment.
Detailed description of the invention
Fig. 1 is the flow diagram for the PVA film that PVA mixed solution preparation of the present invention has polarizing properties；
Fig. 2 is the structural schematic diagram of polaroid of the invention.
Specific embodiment
Embodiment 1
Step 1: Hummers method prepares graphene oxide.2g graphite powder is weighed respectively, pours into the 100ml concentrated sulfuric acid, gradually
10g potassium permanganate is added, is stirred at room temperature 30 minutes.35 DEG C, after constant temperature stirs 2h are adjusted the temperature to again, and 150ml distilled water is added,
It is down to room temperature to solution, hydrogen peroxide is added dropwise to solution in golden yellow.Acquired solution is filtered, centrifugation be washed to it is neutral freeze again it is dry
It is dry to obtain required graphite oxide.
Step 2: graphene quantum dot is prepared.By graphite oxide, high temperature reduction obtains reduction-oxidation graphite under a shielding gas
Alkene.The graphene for weighing 25mg is put into round-bottomed flask, and the 5ml concentrated sulfuric acid and 15ml concentrated nitric acid is added, and is ultrasonically treated 10h.It is added
250ml distilled water is diluted, the acid being then centrifuged in removal solution.Obtained solid is dissolved in the distilled water of 40ml again and being used
Sodium hydroxide solution adjusts PH to 12, then is moved into ptfe autoclave, 200 DEG C of reaction 12h.Obtained graphene quantum
Point is water-soluble and diameter no more than 10nm.
Step 3: PVA film is prepared.Weigh 20g polyvinyl alcohol (PVA) powder, 3g glycerine mixes, be uniformly blended into
30mg graphene quantum dot is placed in 90ml distilled water and 10ml methanol mixed solvent, 80 DEG C of dissolutions stirring 8h, standing and defoaming,
Film forming.
Step 4: PVA film moulding process.With reference to Fig. 1, by PVA film carry out washing swelling, dyeing, extension, correction so that its
With polarized light property.After be respectively placed in 40 DEG C and be respectively dried with 70 DEG C of points of high and low temperature sections.Dyeing, which can be, adsorbs iodine molecule
Can also will have dichromatic organic dyestuff to be adsorbed on PVA on PVA.PVA molecule is originally that any angle is random
Property distribution, under certain temperature and damp condition, stress gradually deflects from force direction after stretching, and be intended to be in line shape point
Cloth.As PVA molecule is arranged in a straight line along draw direction, the iodide ion or dye molecule being adsorbed on PVA layer are also with the side of having
The deflection of tropism, to form long-chain.Bias is played well since iodide ion or dye molecule have, and the row of being parallel to can be absorbed
The polarised light of column direction only allows the polarised light of vertical direction to pass through, to have polarized light property.
Step 5: the compacting of polaroid.According to the structure of Fig. 2, now cellulose triacetate (TAC) film 2, about 4 is pasted
PVA film 3 is closed, then the outer protective film 1 of fitting PET and pressure-sensing glue 5 respectively, is finally bonded release film 6 outside in pressure-sensing glue 5.The polaroid
Suitable for fields such as liquid crystal displays, wherein PVA film with a thickness of 20~60 μm.
Embodiment 2
The preparation of graphene oxide: 1. the 50ml concentrated sulfuric acid and 2g graphite, 1g sodium nitrate are added in beaker and are mixed, in magnetic force
6g potassium permanganate is slowly added under stirring, reaction is placed in 1.5h in ice-water bath.2. reaction temperature is adjusted to after the completion of low-temp reaction
35 DEG C, constant temperature is stirred to react 30min.4. 200ml deionized water after reaction, is slowly added dropwise in medium temperature, it is down to room temperature wait react,
Hydrogen peroxide to solution is added, golden yellow is presented.5. the hydrochloric acid of 10% volume is added, filters, wash away6. after filtering, by filter membrane
On graphite oxide distillation wash and be diluted in beaker, then be centrifuged, PH be washed till neutrality.Freeze-drying 20h must aoxidize stone
Ink.7. dissolving graphite oxide by solvent of distilled water, it is poured on planetary type ball-milling 48h in ball grinder, sufficiently removing expansion carbon-coating, obtained
Graphene oxide.
The preparation of graphene quantum dot: 100mg graphene oxide is dispersed in 30ml water, and 1.2ml concentrated ammonia liquor is added, will
Mixed solution moves in autoclave, is warming up to 300 DEG C of reaction 8h, is cooled to room temperature, and obtained supernatant liquor is separated, i.e.,
Obtain the aqueous dispersions of graphene quantum dot.
The preparation of PVA film: weighing 20g polyvinyl alcohol powder, 3g glycerine mixes, and is uniformly blended into 10mg graphene
Quantum dot is placed in 90ml distilled water and 10ml methanol mixed solvent, and 8h, standing and defoaming, film forming are stirred in 80 DEG C of dissolutions.
The preparation reference implementation example 1 of PVA film molding and polaroid.
Embodiment 3
Graphene oxide is prepared with traditional Hummers method: reference implementation example 1.
The preparation of graphene quantum dot: the nitric acid of the sulfuric acid of 80ml and 30ml are mixed and are added in beaker, is placed the beaker
In ice bath.3g graphene is weighed, graphene is added in beaker while stirring, after two hours, weighs 30gNaClO3,
It is slowly added in mixed solution (this process needs 1h), temperature is avoided to be ramping up and formed suddenly excessive ClO2Gas.When
NaClO3After being completely dissolved, by mixed solution at room temperature strongly stir 48h, by reaction vessels lid loosely cover in order to
Exclude the gas generated.Hereafter, which is stood overnight, the liquid of top 2/3rds is centrifuged at 5000rpm
90min., supernatant liquor pours into beaker, be drop by drop added ammonium hydroxide know PH up to 6-7. then resulting solution put into it is saturating
It analyses bag (8000-14000Da), is placed in 5 days in distilled water and is purified, after 20nm thin film removing large scale piece.Finally, filtrate
It is concentrated with Rotary Evaporators and is freeze-dried to obtain graphene quantum dot powder.
The preparation of PVA film: weighing 20g polyvinyl alcohol powder, 3g glycerine mixes, and is uniformly blended into 45mg graphene
Quantum dot is placed in 90ml distilled water and 10ml methanol mixed solvent, and 8h, standing and defoaming, film forming are stirred in 80 DEG C of dissolutions.
The preparation reference implementation example 1 of PVA film molding and polaroid.
Above-described embodiment is only used to further illustrate a kind of preparation method of PVA film for polaroid of the invention, but
It is to the above embodiments according to the technical essence of the invention any simply to repair the invention is not limited to embodiment
Change, equivalent variations and modification, falls within the scope of protection of technical solution of the present invention.
Claims (10)
1. a kind of preparation method of the PVA film for polaroid, it is characterised in that the following steps are included:
1) graphene quantum dot is prepared, the graphene quantum dot is water-soluble and diameter no more than 10nm；
2) it is uniformly blended into graphene quantum dot after taking PVA powder and plasticizer to mix, is subsequently poured into methanol and distilled water composition
In the mixed solvent, mixed dissolution stirs 6~12h and forms mixed solution at 70 DEG C~90 DEG C, and standing and defoaming simultaneously forms a film；Wherein
PVA powder: plasticizer: methanol: the mass volume ratio of distilled water is 5~40g:0.5~10g:5~20ml:60~120ml, and
Concentration of the graphene quantum dot in mixed solution is 0.1ppm~10ppm；
3) polarized light property is obtained after the PVA film of formation being carried out washing swelling, dyeing, extension and correction, then prior to 30 DEG C
30~90min is dried under~50 DEG C of cryogenic temperature, dries 10~60min then at 60 DEG C~80 DEG C of high-temperature temperature sections.
2. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the graphene amount
Concentration of the son point in mixed solution is 1ppm~5ppm.
3. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the PVA powder:
Plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:5~20ml:60~120ml.
4. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the plasticizer is
Glycerine, the PVA powder: glycerine: methanol: the mass volume ratio of distilled water is 5~40g:1.5~5g:5~20ml:60
~120ml.
5. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: the PVA powder:
Plasticizer: methanol: the mass volume ratio of distilled water is 8~25g:0.5~10g:8~12ml:60~120ml.
6. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: described in step 1)
The preparation method of graphene quantum dot is: graphene being added in the concentrated sulfuric acid and concentrated nitric acid, 5~15h is ultrasonically treated, is then added
The acid that distilled water is diluted and is centrifuged in removal solution, obtained solid are dissolved in the sodium hydroxide solution that pH is 10~13,
It moves into hydrothermal reaction kettle and reacts 10~14h at 180 DEG C~220 DEG C；Wherein graphene: the concentrated sulfuric acid: the quality volume of concentrated nitric acid
Than for 20~30mg:3~8ml concentrated sulfuric acid: 10~20ml concentrated nitric acid.
7. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: described in step 1)
The preparation method of graphene quantum dot is: graphene oxide being dispersed in water, concentrated ammonia liquor mixing is added and moves back to hydro-thermal reaction
In kettle, in 280 DEG C~320 DEG C 6~10h of reaction, supernatant liquor is separated after being cooled to room temperature；Wherein graphene oxide and concentrated ammonia liquor
Ratio be 80~120mg:20~40ml.
8. the preparation method of the PVA film according to claim 1 for polaroid, it is characterised in that: described in step 1)
The preparation method of graphene quantum dot is: sulfuric acid and nitric acid mixed and are placed in ice bath, is added graphene while stirring, 1~
Sodium chlorate is slowly added to after 3h, adition process continues 30min~90min, by mixed solution in room after sodium chlorate is completely dissolved
Temperature is lower to stir 40~60h, is centrifuged the liquid of top 2/3rds after standing overnight to obtain supernatant, adjustment supernatant pH value is extremely
6~7, it is then charged into bag filter and is placed in distilled water and is purified and removed large scale piece, be concentrated and be freeze-dried.
9. a kind of polaroid, it is characterised in that: including PVA film as claimed in any one of claims 1 to 8, cover in PVA film phase
To the TAC film on two sides, cover in the pressure-sensitive of the protective film and another TAC film opposite exterior lateral sides of one of them TAC film opposite exterior lateral sides
Glue.
10. polaroid according to claim 9, it is characterised in that: the polaroid is iodine polarizing piece or dyestuff polarisation
Piece, the PVA film with a thickness of 20~60 μm.
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| CN107012699B (en) * | 2017-03-03 | 2020-05-22 | 厦门祥福兴胶粘制品有限公司 | A kind of manufacturing method of anti-blue light polarizer |
| CN108047662A (en) * | 2017-12-13 | 2018-05-18 | 天津宝兴威科技股份有限公司 | A kind of preparation method of graphene quantum dot enhanced film |
| JP7215160B2 (en) * | 2017-12-28 | 2023-01-31 | 三菱ケミカル株式会社 | POLYVINYL ALCOHOL-BASED FILM FOR PRODUCING POLARIZING FILM, METHOD FOR MANUFACTURING THE SAME, AND POLARIZING FILM |
| CN109655956A (en) * | 2018-12-28 | 2019-04-19 | 昆山之奇美材料科技有限公司 | A kind of polaroid and preparation method thereof with inhibition blue light and moisture-proof function |
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