CN103818070B - White polyester film and preparation method thereof - Google Patents
White polyester film and preparation method thereof Download PDFInfo
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- CN103818070B CN103818070B CN201310683821.5A CN201310683821A CN103818070B CN 103818070 B CN103818070 B CN 103818070B CN 201310683821 A CN201310683821 A CN 201310683821A CN 103818070 B CN103818070 B CN 103818070B
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- white
- antistatic
- polyester film
- master batch
- polyester
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 24
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 37
- 229920000728 polyester Polymers 0.000 claims abstract description 36
- 238000001125 extrusion Methods 0.000 claims abstract description 21
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 46
- 239000000463 material Substances 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 27
- 238000006068 polycondensation reaction Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 18
- 230000032050 esterification Effects 0.000 claims description 17
- 238000005886 esterification reaction Methods 0.000 claims description 17
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052787 antimony Inorganic materials 0.000 claims description 14
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical group [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 14
- -1 wherein Chemical compound 0.000 claims description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 12
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 10
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 10
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims description 10
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 150000001298 alcohols Chemical class 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 239000004408 titanium dioxide Substances 0.000 claims description 9
- 238000004804 winding Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 8
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000010409 thin film Substances 0.000 claims description 8
- 238000004513 sizing Methods 0.000 claims description 7
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 6
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 5
- 238000005453 pelletization Methods 0.000 claims description 5
- 239000011787 zinc oxide Substances 0.000 claims description 5
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 4
- MMEDJBFVJUFIDD-UHFFFAOYSA-N 2-[2-(carboxymethyl)phenyl]acetic acid Chemical compound OC(=O)CC1=CC=CC=C1CC(O)=O MMEDJBFVJUFIDD-UHFFFAOYSA-N 0.000 claims description 3
- ORLQHILJRHBSAY-UHFFFAOYSA-N [1-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1(CO)CCCCC1 ORLQHILJRHBSAY-UHFFFAOYSA-N 0.000 claims description 3
- 239000001361 adipic acid Substances 0.000 claims description 3
- 235000011037 adipic acid Nutrition 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 claims description 3
- 229920005862 polyol Polymers 0.000 claims description 3
- 150000003077 polyols Chemical class 0.000 claims description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 3
- 150000003608 titanium Chemical class 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 150000007942 carboxylates Chemical class 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims 2
- 229910052732 germanium Inorganic materials 0.000 claims 1
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims 1
- 238000002844 melting Methods 0.000 claims 1
- 230000008018 melting Effects 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000002045 lasting effect Effects 0.000 abstract description 2
- 239000012792 core layer Substances 0.000 abstract 3
- 239000002344 surface layer Substances 0.000 abstract 3
- 239000010410 layer Substances 0.000 abstract 2
- 239000004973 liquid crystal related substance Substances 0.000 abstract 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 10
- 239000005020 polyethylene terephthalate Substances 0.000 description 10
- 230000032683 aging Effects 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000000576 coating method Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000004781 supercooling Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000005041 Mylar™ Substances 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- XVZBIIBOLKHMNP-UHFFFAOYSA-N OC(=O)C(O)=O.c1ccc2ccccc2c1 Chemical compound OC(=O)C(O)=O.c1ccc2ccccc2c1 XVZBIIBOLKHMNP-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 150000002290 germanium Chemical class 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001634 Copolyester Polymers 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229940125717 barbiturate Drugs 0.000 description 1
- BUBNOQUZOCSBNU-UHFFFAOYSA-N benzene oxalic acid Chemical compound C1=CC=CC=C1.C(C(=O)O)(=O)O BUBNOQUZOCSBNU-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Landscapes
- Shaping By String And By Release Of Stress In Plastics And The Like (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a white polyester film and a preparation method thereof. The white polyester film comprises a core layer and at least one surface layer, wherein the core layer and the surface layers are obtained by a coextrusion die head extrusion and two-way stretch technology; the core layer is a white polyester layer; each surface layer comprises 70-99.9wt% of pure polyester, 0-30wt% of white master batch and 0.1-10wt% of antistatic master batch. The white polyester film has a lasting antistatic property. The preparation method is simple in technology; an antistatic layer of an obtained product does not fall off; the surface of a film still has the good antistatic property under the conditions of high temperature and humidity; the product is applicable to industries of liquid crystal display, printing and the like.
Description
Technical field
The present invention relates to a kind of white polyester film, particularly to the white polyester film with antistatic property and its system
Preparation Method.
Background technology
Mylar（PET film）It is a kind of comprehensive thin film of Performance comparision, compared with other thermoplastic plastics, it has
Light rate is good, glossy, mechanical performance is excellent, obdurability and the advantages of impact strength, and dimensionally stable.White polyester film
Due to high brightness, reflection characteristic and excellent disguise advertisement tag, image show and print etc. that aspect has a uniqueness should
With particularly in flat pannel display industry, indispensable as the reflectance coating of backlight module.
In the production process of white polyester film, because the reasons such as friction make thin film produce electrostatic, the thin film with electrostatic
It is applied to easily because static discharge makes backlight module impaired during backlight module, the integrated circuit of infringement backlight module, light-emitting diodes
Pipe or CCFL, therefore, in order to prevent the generation of these problems, for white polyester film, then require it to have
Anlistatig performance.
Generally, for giving white polyester film antistatic property, the method generally adopting is on white polyester film surface
Coating antistatic layer, but the method for this coating suffers from the drawback that：（1）Technique is complex, increases production cost；（2）By
It is that reflectance coating surface is sticked to by binding agent in antistatic layer, in some specific environments（As hot and humid, low temperature and low humidity
Etc. extreme condition）, antistatic layer is easy to fall off, does not have anlistatig effect；（3）The table of thin film in coating process, can be made
Sight occurs being unevenly coated, the disadvantage such as produces bar road, grows dim.
Content of the invention
The technical problem to be solved in the present invention is for the deficiencies in the prior art, provides a kind of white polyester film, its tool
There is lasting antistatic property.
The invention solves the problems that another technical problem be that a kind of preparation method of white polyester film is provided.
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows：
A kind of white polyester film, including sandwich layer and at least one of which top layer it is characterised in that described sandwich layer and top layer are through altogether
Ji die head extrusion and stretch processes and obtain, sandwich layer is white polyester layer, and the pure poly- of 70wt% ~ 99.9wt% is contained on top layer
The antistatic master batch of ester, the white master material of 0wt% ~ 30wt% and 0.1wt% ~ 10wt%.
Above-mentioned white polyester film, described sandwich layer contains the clear polyester of 20wt% ~ 75wt% and the white of 25wt% ~ 80wt%
Masterbatch.
Above-mentioned white polyester film, described white master material is by the clear polyester of 30wt% ~ 70 wt %, 15 wt % ~ 60
The Calcium Carbonate of the titanium dioxide of wt % and 0 wt % ~ 10 wt %, barium sulfate, zinc oxide or zirconium oxide composition, by twin-screw extrusion
Pelletize obtains.
Above-mentioned white polyester film, described antistatic master batch is prepared by following methods：
（1）Esterification process：
Add binary acid, dihydroxylic alcohols and catalyst in consersion unit, be passed through nitrogen protection, in 220 DEG C ~ 270 DEG C of bar
Esterification 3 ~ 4 hours under part；
（2）Polycondensation process：
After esterification, add antistatic additive in esterification system, after consersion unit evacuation, 265 DEG C ~ 290
Carry out polycondensation reaction 3-5 hour under conditions of DEG C, obtain polycondensation products；
（3）Granulation process：
Polycondensation product is through making silk, cooling, cutting, prepared biaxially oriented polyester film antistatic master batch.
Above-mentioned white polyester film, described binary acid be selected from p-phthalic acid, to phenylenediacetic Acid, naphthalenedicarboxylic acid, to naphthalene two
Acetic acid, adipic acid, SA, M-phthalic acid, phthalic acid.
Above-mentioned white polyester film, described dihydroxylic alcohols are aliphatic diol that carbon number is 2 ~ 4.
Above-mentioned white polyester film, described dihydroxylic alcohols be selected from ethylene glycol, propylene glycol, butanediol, 1,3-PD, Isosorbide-5-Nitrae-
Butanediol, cyclohexanedimethanol.
Above-mentioned white polyester film, described catalyst is selected from antimony-based catalyst, germanium series catalysts and Titanium series catalyst
One or two.
Above-mentioned white polyester film, described catalyst is antimony glycol, and wherein, content in antistatic master batch for the antimony is
0.001wt%~0.05wt%.
Above-mentioned white polyester film, described antistatic additive is selected from amine salt, quaternary ammonium salt, metal carboxylate, Sulfonateses, phosphorus
Acid esters type, polyol type one or two；
The addition of described antistatic additive is the 1wt% ~ 20wt% of antistatic master batch gross weight.
Above-mentioned white polyester film, the intrinsic viscosity of described antistatic master batch is 0.50dL/g ~ 0.80dL/g.
A kind of preparation method of white polyester film, it comprises the steps：
（1）Melt extrude：Clear polyester and white master material are mixed in proportion in feeding single screw extrusion machine and melt,
Antistatic master batch, white master material, clear polyester are mixed in proportion in feeding double screw extruder and melt, melt passes through altogether
Extrusion die head is extruded；
（2）Cooling slab：Melt forms unformed polyester casting sheet on the chill roll rotating；
（3）Biaxial tension：After sheet is preheated, 3.0 ~ 4.4 times of longitudinal stretching, then carry out 2.5 ~ 4.5 times of cross directional stretch；
（4）Sizing winding：Thin film after biaxial tension is carried out thermal finalization, then cools down winding, obtain white antistatic and gather
Ester film.
Above-mentioned preparation method, described melt temperature is 260 DEG C ~ 300 DEG C；Described heat setting temperature is 200 DEG C ~ 240 DEG C.
Compared with prior art, the invention has the advantages that：
The present invention passes through the co-extrusion die head extrusion and stretch processes using sandwich layer and top layer, and by controlling in top layer
The content of each component, makes antistatic additive being evenly distributed in the film, antistatic property persistently, solve simultaneously coating process to
Thin film apparent cause be unevenly coated, the quality drawback such as produce bar road, grow dim, improve the quality of product.The present invention provides
Preparation method process is simple, the antistatic layer of the product obtaining do not fall off, and under the conditions of hot and humid, film surface still has
Good antistatic property.
Specific embodiment
In the present invention, described sandwich layer, the clear polyester on top layer are the polymer that binary acid and dihydroxylic alcohols are obtained by polycondensation,
Wherein binary acid includes p-phthalic acid, to phenylenediacetic Acid, to naphthalene oxalic acid, M-phthalic acid, phthalic acid etc., preferred pair
Phthalic acid, also can add a small amount of M-phthalic acid class modified copolyester；Dihydroxylic alcohols are aliphatic two that carbon number is 2 ~ 4
Alcohol, including ethylene glycol, propylene glycol, butanediol, 1,3-PD etc., preferably ethylene glycol.The clear polyester of the suitable present invention is poly-
Ethylene glycol terephthalate, its intrinsic viscosity is 0.55dL/g ~ 0.95dL/g, preferably 0.60dL/g ~ 0.75dL/g.
In the present invention, in described sandwich layer, top layer, white master material is made up of clear polyester and inorganic particulate, is squeezed by twin screw
Go out pelletize to be obtained, wherein inorganic particulate can be in titanium dioxide, barium sulfate, zinc oxide, zirconium oxide, aluminium oxide, Calcium Carbonate
One or more it is contemplated that the whiteness of mylar, light stability and reflectance etc. require, preferable particle size is 0.1 ~ 10 μm
Titanium dioxide, can mix a little Calcium Carbonate, barium sulfate, zinc oxide or zirconium oxide.
In the present invention, the antistatic master batch in top layer is prepared by following methods：
（1）Esterification process：
Add binary acid, dihydroxylic alcohols and catalyst in consersion unit, be passed through nitrogen protection, in 220 DEG C ~ 270 DEG C of bar
Esterification 3 ~ 4 hours under part；Wherein, binary acid can with identical in clear polyester, can selected from p-phthalic acid, to benzene
Oxalic acid, naphthalenedicarboxylic acid, to naphthalene oxalic acid, adipic acid, SA, M-phthalic acid, phthalic acid；Dihydroxylic alcohols are carbon atom
Number is 2 ~ 4 aliphatic diol, and it can be identical with clear polyester, such as ethylene glycol, propylene glycol, butanediol, 1,3-PD,
1,4- butanediol, cyclohexanedimethanol；Catalyst can be selected from antimony-based catalyst, germanium series catalysts and Titanium series catalyst
Plant or two kinds, when preferred catalyst is antimony glycol, content in antistatic master batch for the antimony is 0.001wt% ~ 0.05wt%.
（2）Polycondensation process：
After esterification, add antistatic additive in esterification system, after consersion unit evacuation, 265 DEG C ~ 290
Carry out polycondensation reaction 3-5 hour under conditions of DEG C, obtain polycondensation products；Antistatic additive can be selected from amine salt, quaternary ammonium salt, carboxylic
Barbiturates, Sulfonateses, phosphate type, polyol type one or two, the addition of antistatic additive is that antistatic master batch is total
1wt% ~ the 20wt% of weight.
（3）Granulation process：
Polycondensation product is through making silk, cooling, cutting, prepared biaxially oriented polyester film antistatic master batch.Described antistatic
The intrinsic viscosity of masterbatch is 0.50dL/g ~ 0.80dL/g.
With reference to specific embodiment, the present invention is specifically described, but the invention is not limited in this.
Embodiment 1
1. the preparation of antistatic master batch
Add 15kg p-phthalic acid, 7.85kg ethylene glycol and 0.21g antimony glycol in reactor, nitrogen is protected,
Carry out esterification under the conditions of 265 DEG C after 3 hours, add 1.2kg hexadecyltrimethylammonium chloride in reactor, to reaction
Kettle carries out evacuation, and keeps temperature in the kettle to carry out polycondensation reaction 3h under conditions of being 280 DEG C；Terminate polycondensation reaction, through make silk,
Cooling, cutting, obtain intrinsic viscosity be 0.55dL/g, weight be 18.54kg antistatic master batch, the wherein content of antistatic additive
For 6.9wt%, standby.
2. the preparation of white master material
By the clear polyester drying and crushing of 30g, then mix with the titanium dioxide of 60g, the Calcium Carbonate of the zirconium oxide 5g of 5g
Uniformly, through double screw extruder extruding pelletization, make white master material, standby.
3. the preparation of white polyester film
The polyethylene terephthalate polyester for 0.65dL/g for the intrinsic viscosity is cut into slices and above-mentioned white master material, according to
75%:25% weight, than mix homogeneously, is sent into single screw extrusion machine, is melt extruded under the conditions of 270 DEG C.
By the polyethylene terephthalate polyester section for 0.60dL/g for the intrinsic viscosity, above-mentioned white master material and anti-
Electrostatic masterbatch, according to 83%:10%:7% weight, than mix homogeneously, sends into double screw extruder, melts and squeeze under the conditions of 275 DEG C
Go out.
Above two fused materials are passed through a co-extrusion die head, melt is cast on the chill roll of a rotation, become no
The casting sheet of the A/B/A three-decker of sizing.
After this casting sheet is preheated, successively longitudinal stretching multiple is carried out with 4.0 multiplying power and carry out longitudinal stretching, with 3.0
Multiplying power carry out cross directional stretch, polymeric film thermal finalization under about 220 DEG C of temperature conditionss that biaxial tension is orientated, final warp
The processes such as supercooling, winding, obtain white polyester film, test optical property before and after its hydrothermal aging, antistatic property.
Embodiment 2
1. the preparation of antistatic master batch
Add 10kg p-phthalic acid, 5.21kg ethylene glycol and 3.83g antimony glycol in reactor, nitrogen is protected,
Carry out esterification under the conditions of 250 DEG C after 3.5 hours, add the hexadecyltrimethylammonium chloride of 1.12kg in reactor,
Evacuation is carried out to reactor, and keeps temperature in the kettle to carry out polycondensation reaction 3.5h under conditions of being 285 DEG C；Terminate polycondensation anti-
Should, through making silk, cooling, cutting, prepared intrinsic viscosity is 0.60dL/g, and weight is the antistatic master batch of 12.68kg, wherein anti-quiet
The content of electric agent is 9.7wt%, standby.
2. the preparation of white master material
By the clear polyester drying and crushing of 78g, then mix homogeneously with the titanium dioxide of 15g and the zinc oxide of 7g, through double
Screw extruder extruding pelletization, makes white master material, standby.
3. the preparation of white polyester film
The polyethylene terephthalate polyester for 0.80dL/g for the intrinsic viscosity is cut into slices and above-mentioned white master material, according to
20%:70% weight sends into single screw extrusion machine than mix homogeneously, melt extrudes under the conditions of 275 DEG C.
By the polyethylene terephthalate polyester section for 0.55dL/g for the intrinsic viscosity, above-mentioned white master material and anti-
Electrostatic masterbatch, according to 70%:28%:2% weight, than mix homogeneously, sends into double screw extruder, melts and squeeze under the conditions of 285 DEG C
Go out.
Above two fused materials are passed through a co-extrusion die head, melt is cast on the chill roll of a rotation, become no
The casting sheet of the A/B/A three-decker of sizing.
After this casting sheet is preheated, successively longitudinal stretching multiple is carried out with 3.0 multiplying power and carry out longitudinal stretching, with 4.5
Multiplying power carry out cross directional stretch, polymeric film thermal finalization under about 225 DEG C of temperature conditionss that biaxial tension is orientated, final warp
The processes such as supercooling, winding, obtain white polyester film, test optical property before and after its hydrothermal aging, antistatic property.
Embodiment 3
1. the preparation of antistatic master batch
Add 8kg p-phthalic acid, 4.17kg ethylene glycol and 3.22g antimony glycol in reactor, nitrogen is protected,
Carry out esterification under the conditions of 266 DEG C after 3 hours, add the hexadecyltrimethylammonium chloride of 1.80kg in reactor, right
Reactor carries out evacuation, and keeps temperature in the kettle to carry out polycondensation reaction 3.5h under conditions of being 283 DEG C；Terminate polycondensation reaction,
Through making silk, cooling, cutting, prepared intrinsic viscosity is 0.66dL/g, and weight is the antistatic master batch of 11.05kg, wherein antistatic
The content of agent is 19.5wt%, standby.
2. the preparation of white master material
By the clear polyester drying and crushing of 60g, then mix homogeneously with the titanium dioxide of 40g, squeeze through double screw extruder
Go out pelletize, make white master material, standby.
3. the preparation of white polyester film
The polyethylene terephthalate polyester for 0.55dL/g for the intrinsic viscosity is cut into slices and above-mentioned white master material, according to
60%:40% weight sends into single screw extrusion machine than mix homogeneously, melt extrudes under the conditions of 285 DEG C.
By the polyethylene terephthalate polyester section for 0.80dL/g for the intrinsic viscosity, above-mentioned white master material and anti-
Electrostatic masterbatch, according to 99.9%:0.1% weight, than mix homogeneously, sends into double screw extruder, melts and squeeze under the conditions of 290 DEG C
Go out.
Above two fused materials are passed through a co-extrusion die head, melt is cast on the chill roll of a rotation, become no
The casting sheet of the A/B/A three-decker of sizing.
After this casting sheet is preheated, successively longitudinal stretching multiple is carried out with 3.3 multiplying power and carry out longitudinal stretching, with 3.5
Multiplying power carry out cross directional stretch, polymeric film thermal finalization under about 230 DEG C of temperature conditionss that biaxial tension is orientated, final warp
The processes such as supercooling, winding, obtain white polyester film, test optical property before and after its hydrothermal aging, antistatic property.
Embodiment 4
1. the preparation of antistatic master batch
Add 5kg p-phthalic acid, 2.60kg ethylene glycol and 2.88g antimony glycol in reactor, nitrogen is protected,
Carry out esterification under the conditions of 255 DEG C after 4 hours, add the hexadecyltrimethylammonium chloride of 0.86kg in reactor, right
Reactor carries out evacuation, and keeps temperature in the kettle to carry out polycondensation reaction 4h under conditions of being 288 DEG C；Terminate polycondensation reaction, warp
Make silk, cooling, cutting, prepared intrinsic viscosity is 0.70dL/g, the antistatic master batch for 6.64kg for the weight, wherein antistatic additive
Content is 14.9wt%, standby.
2. the preparation of white master material
By the clear polyester drying and crushing of 45g, then mix homogeneously with the titanium dioxide of 50g and the barium sulfate of 5g, through double
Screw extruder extruding pelletization, makes white master material, standby.
3. the preparation of white polyester film
The polyethylene terephthalate polyester for 0.65dL/g for the intrinsic viscosity is cut into slices and above-mentioned white master material, according to
75%:35% weight sends into single screw extrusion machine than mix homogeneously, melt extrudes under the conditions of 280 DEG C.
By the polyethylene terephthalate polyester section for 0.65dL/g for the intrinsic viscosity, above-mentioned white master material and anti-
Electrostatic masterbatch, according to 80%:17%:3% weight, than mix homogeneously, sends into double screw extruder, melts and squeeze under the conditions of 290 DEG C
Go out.
Above two fused materials are passed through a co-extrusion die head, melt is cast on the chill roll of a rotation, become no
The casting sheet of the A/B/A three-decker of sizing.
After this casting sheet is preheated, successively longitudinal stretching multiple is carried out with 3.1 multiplying power and carry out longitudinal stretching, with 3.0
Multiplying power carry out cross directional stretch, polymeric film thermal finalization under about 235 DEG C of temperature conditionss that biaxial tension is orientated, final warp
The processes such as supercooling, winding, obtain white polyester film, test optical property before and after its hydrothermal aging, antistatic property.
Embodiment 5
1. the preparation of antistatic master batch
Add 20kg p-phthalic acid, 10.42kg ethylene glycol and 7.26g antimony glycol in reactor, nitrogen is protected,
Carry out esterification under the conditions of 270 DEG C after 3 hours, add the hexadecyltrimethylammonium chloride of 0.24kg in reactor, right
Reactor carries out evacuation, and keeps temperature in the kettle to carry out polycondensation reaction 4.5h under conditions of being 278 DEG C；Terminate polycondensation reaction,
Through making silk, cooling, cutting, prepared intrinsic viscosity is 0.75dL/g, and weight is the antistatic master batch of 23.36kg, wherein antistatic
The content of agent is 1wt%.
2. the preparation of white master material
By the clear polyester drying and crushing of 40g, then mix homogeneously with the titanium dioxide of 30g and the zirconium oxide of 6g, through double
Screw extruder extruding pelletization, makes white master material, standby.
3. the preparation of white polyester film
The polyethylene terephthalate polyester for 0.67dL/g for the intrinsic viscosity is cut into slices and above-mentioned white master material, according to
50%:50% weight sends into single screw extrusion machine than mix homogeneously, melt extrudes under the conditions of 265 DEG C.
By the polyethylene terephthalate polyester section for 0.67dL/g for the intrinsic viscosity, above-mentioned white master material and anti-
Electrostatic masterbatch, according to 60%:30%:10% weight, than mix homogeneously, sends into double screw extruder, melts and squeeze under the conditions of 280 DEG C
Go out.
Above two fused materials are passed through a co-extrusion die head, melt is cast on the chill roll of a rotation, become no
The casting sheet of the A/B/A three-decker of sizing.
After this casting sheet is preheated, successively longitudinal stretching multiple is carried out with 3.5 multiplying power and carry out longitudinal stretching, with 3.8
Multiplying power carry out cross directional stretch, polymeric film thermal finalization under about 225 DEG C of temperature conditionss that biaxial tension is orientated, final warp
The processes such as supercooling, winding, obtain white polyester film, test optical property before and after its hydrothermal aging, antistatic property.
Table one：Optical property and antistatic property contrast before and after hydrothermal aging
In table, the method for testing of properties is as follows：
1st, light transmittance, mist degree：According to ASTM D1003 test；
2nd, surface resistivity：According to ASTM D257 standard testing；
3rd, hydrothermal aging performance：With reference to ASTM D257 standard, wherein print is in 65 DEG C of temperature, constant temperature under the conditions of humidity 90%
Constant humidity 500h.
Data from table 1 can be seen that the white polyester film surface resistivity obtaining using technical solution of the present invention
Less than 1E+10 Ω；After hydrothermal aging, its antistatic property is still preferable.
Claims (8)
1. a kind of white polyester film, including sandwich layer and at least one of which top layer it is characterised in that described sandwich layer and top layer are through co-extrusion
Die head extrusion and stretch processes and obtain, sandwich layer be white polyester layer, the pure of 70wt%～99.9wt% is contained on top layer
The antistatic master batch of polyester, the white master material of 0wt%～30wt% and 0.1wt%～10wt%, the content sum of each component is
100wt%；
Described antistatic master batch is prepared by following methods：
(1) esterification process：
Add binary acid, dihydroxylic alcohols and catalyst in consersion unit, be passed through nitrogen protection, under conditions of 220 DEG C～270 DEG C
Esterification 3～4 hours；
(2) polycondensation process：
After esterification, add antistatic additive in esterification system, after consersion unit evacuation, at 265 DEG C～290 DEG C
Under the conditions of carry out polycondensation reaction 3-5 hour, obtain polycondensation products；
(3) granulation process：
Polycondensation product is through making silk, cooling, cutting, prepared biaxially oriented polyester film antistatic master batch；
The intrinsic viscosity of described antistatic master batch is 0.50dL/g～0.80dL/g；
Described white master material by the clear polyester of 30wt%～85wt%, the titanium dioxide of 15wt%～60wt% and 0wt%～
The Calcium Carbonate of 10wt%, barium sulfate, zinc oxide or zirconium oxide composition, are obtained by double-screw extruding pelletizing；
The addition of described antistatic additive is the 1wt%～20wt% of antistatic master batch gross weight.
2. white polyester film according to claim 1 is it is characterised in that described sandwich layer contains 20wt%～75wt%'s
Clear polyester and the white master material of 25wt%～80wt%.
3. white polyester film according to claim 2 is it is characterised in that described binary acid is selected from p-phthalic acid, right
Phenylenediacetic Acid, naphthalenedicarboxylic acid, adipic acid, SA, M-phthalic acid, phthalic acid；
Described dihydroxylic alcohols are selected from ethylene glycol, propylene glycol, butanediol, 1,3- propylene glycol or cyclohexanedimethanol.
4. white polyester film according to claim 3 is it is characterised in that described catalyst is selected from antimony-based catalyst, germanium
One of series catalysts and Titanium series catalyst or two kinds.
5. white polyester film according to claim 4 is it is characterised in that described catalyst is antimony glycol, wherein, antimony
Content in antistatic master batch is 0.001wt%～0.05wt%.
6. white polyester film according to claim 5 is it is characterised in that described antistatic additive is selected from amine salt, quaternary ammonium
Salt, metal carboxylate, Sulfonateses, phosphate type, polyol type one or two.
7. a kind of method preparing white polyester film as any one of claim 1～6 it is characterised in that include as
Lower step：
(1) melt extrude：Clear polyester and white master material are mixed in proportion in feeding single screw extrusion machine and melts, will resist
Electrostatic masterbatch, white master material, clear polyester mix in proportion melting in feeding double screw extruder, and melt passes through coextruding die
Head extrusion；
(2) cool down slab：Melt forms unformed polyester casting sheet on the chill roll rotating；
(3) biaxial tension：After sheet is preheated, 3.0～4.4 times of longitudinal stretching, then carry out 2.5～4.5 times of cross directional stretch；
(4) sizing winding：Thin film after biaxial tension is carried out thermal finalization, then cools down winding, obtain white antistatic polyester thin
Film.
8. method according to claim 7 is it is characterised in that melt temperature is 260 DEG C～300 DEG C.
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| CN105500856B (en) * | 2015-12-15 | 2018-02-27 | 哈尔滨工业大学无锡新材料研究院 | Can be with the directly hot composite polyester film of engineering plastics and preparation method thereof |
| CN107556707A (en) * | 2017-08-22 | 2018-01-09 | 界首市天鸿新材料股份有限公司 | A kind of fire retardant insulating polyester film and its production technology |
| CN111703167B (en) * | 2020-06-28 | 2021-04-27 | 广东裕泰实业有限公司 | High-antistatic modified polymer insulating material and preparation method thereof |
| CN117004064B (en) * | 2023-08-14 | 2024-02-20 | 广东宝佳利新材料股份有限公司 | Special polyester film for shallow screen printing and preparation process thereof |
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|---|---|---|---|---|
| EP1125970A1 (en) * | 2000-02-19 | 2001-08-22 | Mitsubishi Polyester Film GmbH | White opaque film with low transparency made from a crystallizable thermoplastic and having additional functionality |
| WO2008053740A1 (en) * | 2006-10-27 | 2008-05-08 | Toray Industries, Inc. | White polyester film for liquid crystal display reflector |
| CN101318393A (en) * | 2008-07-08 | 2008-12-10 | 常州裕兴绝缘材料有限公司 | Electrostatic resistant heavy duty polyester film and method of preparing the same |
| CN102371743A (en) * | 2011-08-29 | 2012-03-14 | 合肥乐凯科技产业有限公司 | Antistatic polyester film and preparation method thereof |
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|---|---|---|---|---|
| JP2007298963A (en) * | 2006-04-07 | 2007-11-15 | Toray Ind Inc | White polyester film for liquid crystal reflector, and surface light source using the film |
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2013
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|---|---|---|---|---|
| EP1125970A1 (en) * | 2000-02-19 | 2001-08-22 | Mitsubishi Polyester Film GmbH | White opaque film with low transparency made from a crystallizable thermoplastic and having additional functionality |
| WO2008053740A1 (en) * | 2006-10-27 | 2008-05-08 | Toray Industries, Inc. | White polyester film for liquid crystal display reflector |
| CN101318393A (en) * | 2008-07-08 | 2008-12-10 | 常州裕兴绝缘材料有限公司 | Electrostatic resistant heavy duty polyester film and method of preparing the same |
| CN102371743A (en) * | 2011-08-29 | 2012-03-14 | 合肥乐凯科技产业有限公司 | Antistatic polyester film and preparation method thereof |
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