CN103102474B - Matt polyester film preparation method - Google Patents
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- CN103102474B CN103102474B CN201110353645.XA CN201110353645A CN103102474B CN 103102474 B CN103102474 B CN 103102474B CN 201110353645 A CN201110353645 A CN 201110353645A CN 103102474 B CN103102474 B CN 103102474B
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Abstract
The invention discloses a matt polyester film preparation method, which comprises that: a dibasic acid, a dihydric alcohol and an additive dispersion liquid are subjected to an esterification reaction under an effect of a catalyst; a stabilizer is added to carry out a condensation polymerization reaction to obtain a matt film polyester; the matt film polyester is subjected to drying, melt extrusion at a temperature of 270-290 DEG C, vertical and horizontal double direction stretching, heat shaping, relaxing, cooling, traction and rolling to prepare the matt polyester film having a single layer or multi-layer structure, wherein the vertical and horizontal double direction stretching is performed at a temperature of 80-120 DEG C and under a stretching ratio of 3.0-4.0:1, the additive in the additive dispersion liquid comprises 60-80% by mass of kaolin and 40-20% by mass of barium sulfate, and an average particle size of the additive is 0.3-0.5 mum. Compared to the conventional polyester film, the matt polyester film prepared by the method has a good matt effect, wherein 45 DEG gloss is less than 30%.
Description
Technical field
The invention belongs to field of polymer chemical industry, be specifically related to a kind of preparation of matt polyester film.
Background technology
Two-way stretch pet film (being called for short BOPET), has excellent physical and chemical performance, can be widely used in numerous areas.Packaging industry has very large demand to the biaxially oriented polyester film of high transparency, high gloss all the time, because it can make packing list mask gloss and magnetism.Correspond, the sub-optical thin film of low-luster can make surface of package have more dim sense and artistry, the desire to purchase more stimulated consumer, sub-light film is except having the superior chemical physics performance of conventional polyester film, mainly also have: haze, the features such as low gloss, have and aluminize preferably and printing performance.Sub-light film is applicable to the overlay film application etc. of the printing packagings such as the making of the special high-grade label such as household electrical appliance, computer precision plant and instrument, indoor sub-light finishing material and high-grade cigarette, wine, high-grade books.
For reducing polyester film glossiness, more people is studied work, and these researchs mainly contain:
Chinese patent 200810015273.8 discloses a kind of single-face matt polyester film, and this patent adopts does not prepare master batch in advance, and the method adding nylon superpolymer and crystallization nucleation auxiliary agent when masking prepares sub-optical thin film.Adding crystallization nucleating agent when masking can cause film crystal unity excessive, occurs that not easily stretching and additive disperse uneven drawback.
Chinese patent 200410039196.1 discloses light tight sub-smooth type polyester film of a kind of black and preparation method thereof, this patent polyester film is by (1) sub-light polyester slice, (2) carbon black type black polyester masterbatch, (3) the compound black polyester masterbatch composition of carbon black organic dye, this patent adopts blending method to prepare sub-optical thin film, and additive is not easily uniformly dispersed in the film.
Chinese patent 200810044519.4 discloses a kind of manufacture method of transparent suboptical polyester film, and this patent adopts sub-for acrylic clear photopolymer resin and solvent, is mixed with the sub-photopolymer resin solution of acrylic clear; Again sub-for acrylic clear photopolymer resin solution is coated on polyester film through coating process, obtained transparent suboptical polyester film.This patent coating method prepares sub-optical thin film, requires higher to masking, coating apparatus.
Chinese patent 200410016500.0 discloses a kind of polyester film and production method thereof of at least single-face matt, and this patent adopts interpolation nano silicon and micron silica to make master batch, then prepares sub-optical thin film.Wherein nano silicon is more difficult is uniformly dispersed.
Method is put in the preparation that Chinese patent 200810020898.3 discloses a kind of polyester for low-haze biaxial stretching polyester film, this patent adopts that to add median size be that the kaolin of 1.0 ~ 4.0 μm or barium sulfate synthesize polyester for film as caking inhibiter, to reduce polyester mist degree, caking inhibiter add-on is 800 ~ 3500ppm of polyester quality.The present invention adds the mixture of kaolin and barium sulfate, its addition is the 1-5% of polyester quality, if kaolin and barium sulfate median size are 0.3 ~ 0.5 μm. be that the kaolin of 1.0 ~ 4.0 μm or barium sulfate do additive by median size, add-on is all the 1-5% of polyester quality, the film surface so made is very coarse, frictional coefficient is very large, then it is very difficult to carry out the processing of rear road.And add the slightly smaller additive of median size, add equal in quality additive, the additive number that median size is little is many, plays the effect of nucleator on the one hand, and crystallizing polyester degree increases, and affects refractive index.On the other hand, add equal in quality additive, the film friction coefficient made of the additive that median size is little is corresponding to diminish, and is conducive to rear road and processes.
Summary of the invention
The present invention is from affecting film glossiness principle, add in the polymerization process of direct esterification synthesizing polyester by selecting suitable additive, obtained sub-light polyester for film, this polyester drying is extruded drawing and setting and is made matt polyester film, compared with normal polyester film, there is good matt effect.Sub-light polyester for film, when preparing film, can be used as master batch and adds or be directly used in the sub-optical thin film of preparation, need not add other caking inhibiters again.
Object of the present invention can be reached by following measures:
The preparation method of matt polyester film: diprotic acid, dibasic alcohol, additive dispersion liquid are first carried out an esterification under the effect of catalyzer, then add stablizer and carry out polycondensation, obtain sub-light polyester for film; This sub-light polyester for film melt extrudes through super-dry, at 270 ~ 290 DEG C, and in temperature 80 ~ 120 DEG C, stretching ratio 3.0 ~ 4.0: 1 time two-way stretch in length and breadth, heat setting type again, lax, cooling, traction, rolling, make the matt polyester film of single or multiple lift structure; The thickness of this matt polyester film is 20 ~ 100 μm, and 45 degree of glossiness of matt polyester film prepared by this law are less than 30%.
In additive dispersion liquid of the present invention, described additive is made up of extra fine quality content 60 ~ 80% kaolin and 40 ~ 20% barium sulfate, and the median size of this additive need within the scope of 0.3 ~ 0.5 μm, and the dispersion solvent of additive dispersion liquid is dibasic alcohol.The consumption of additive is 1 ~ 5% of polyester quality.Additive dispersion liquid generally needs, first through high speed dispersion or with granulated glass sphere grinding, to make it be dispersed in EG, then join in polyester synthetic system.The mass concentration of additive dispersion liquid is 20 ~ 60%, preferably 25 ~ 35%.Additive, in grinding distribution process, can add dispersion agent, and dispersion agent is sodium polyphosphate or potassium polyphosphate, and its add-on is relative to the additive quality be applicable to 0.1% ~ 0.5%.
Sub-light polyester for film of the present invention is with diprotic acid and dibasic alcohol for main raw material, and adopt direct esterification to produce polyester, preparation process comprises esterification and polycondensation.Applicable additive, catalyzer and stablizer is added when reacting.Wherein esterification temperature is 210 ~ 280 DEG C, and absolute pressure is 0.1 ~ 0.5MPa, and esterification time is 1 ~ 5 hour; Condensation temperature is 250 ~ 295 DEG C, polycondensation absolute pressure≤1KPa, and the reaction times is 0.5 ~ 4 hour, and through pelletizing, drying, obtained polyester slice, the limiting viscosity of gained polyester slice is 0.55 ~ 0.70dl/g.
Diprotic acid in this law is terephthalic acid, particularly PTA or QTA, and described dibasic alcohol is the dibasic alcohol of EG class, particularly ethylene glycol, and wherein diprotic acid is 1: 1.2 ~ 1: 2.0 with the ratio of the molar weight of ethylene glycol.The polyester obtained is the homopolymer of polyester, or multipolymer.
The catalyzer of present method is germanium, antimony or titanium class catalyzer, comprises mineral compound or their organic complex of germanic, antimony or titanium, concrete as antimony glycol, antimony acetate, germanium dioxide etc.The consumption of catalyzer is 0.01 ~ 0.09% of polyester quality.
Described stablizer is phosphoric acid, phosphorous acid, Tripyrophosphoric acid, trimethyl phosphite 99, triphenylphosphate or triethyl phosphate, and the consumption of described stablizer is 0.0003 ~ 0.040% of polyester quality.
In the preparation of polyester film, the temperature of its sizing is 180 DEG C-230 DEG C, and shaping time is 1 ~ 3 second.Sub-light polyester for film can be independent raw material, also can be used in combination with other raw materials, need not add other caking inhibiters again.The preparation of polyester film more specifically step comprise sub-light polyester for film pre-crystallized, dry, melt extrude, in length and breadth to steps such as two-way stretch, heat setting type, lax, cooling, traction, rollings.Pre-crystallized step is same as the prior art, and it generally carries out at 110 ~ 150 DEG C.The mode of drying step adopts bleeds or hot gas flow is carried secretly.Dry section obtains sheet through melt extruding again, and extrusion temperature is 270 ~ 290 DEG C.The stretching ratio of sheet in biaxial orientation process in length and breadth 3.0 ~ 4.0: 1 (namely vertical draw multiplying power to be 3.0 ~ 4.0: 1, horizontal multiplying power of drawing is 3.0 ~ 4.0: 1), draft temperature 80 ~ 120 DEG C.Heat setting type adopts temperature 180 DEG C ~ 230 DEG C and 1 ~ 3 second time.
The present invention filters out applicable additive and additive formula by great many of experiments, i.e. kaolin 60 ~ 80%+ barium sulfate 40 ~ 20%, if add kaolin to be greater than 90%, 0.3-0.5 μm of kaolin is difficult to be uniformly dispersed, if add barium sulfate to be greater than 40%, the glossiness making film improves, and does not reach matt effect.The present invention adds in the course of the polymerization process by after the dispersion of the additive of the suitable proportioning of screening, obtained sub-light polyester for film, and under specific film forming condition, this polyester can be used as master batch interpolation or is directly used in and prepares film, need not add other caking inhibiters again.With the matt polyester film that this sub-light polyester for film is made for raw material, compared with normal polyester film, have good matt effect, its 45 degree of glossiness are less than 30%.
Embodiment
Embodiment 1
In sand mill, add 400ml granulated glass sphere, 140g kaolin, 60g barium sulfate, 600g ethylene glycol, 0.3g sodium polyphosphate, grind 1 hour, prepare kaolin-barium sulfate-glycolic suspension, wherein kaolin-barium sulfate median size 0.32 μm.
5.0Kg PTA is added in 20L typical zolymerization reactor, 3KgEG, 2.0g antimony acetate, the above-mentioned kaolin-barium sulfate-glycolic suspension of 278g, 230 ~ 265 DEG C, carry out esterification under 0.2 ~ 0.3Mpa (gauge pressure), when aquifer yield reaches 1200ml, pressure release, to normal pressure, adds 1.025g triphenylphosphate, atmospheric agitation 10 minutes, intensification degree of falling is pressed onto 280 DEG C and below 100Pa, reacts 1 ~ 3 hour.React complete and extrude through Melt Pump, pelletizing, drying, obtain the sub-light polyester film section that limiting viscosity is 0.650dl/g.
By obtained sub-light polyester for film section through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cool, make 70 μm of single thin films.Wherein extrusion temperature is 275 ~ 285 DEG C, and vertical La Wendu is 105 DEG C, and horizontal La Wendu is 105 DEG C, and vertical multiplying power of drawing is: 3.0: 1, and horizontal multiplying power of drawing is: 3.0: 1, setting temperature 220 DEG C, shaping time 1 second.
Embodiment 2
In sand mill, add 400ml granulated glass sphere, 182g kaolin, 98g barium sulfate, 520g ethylene glycol, 0.7g potassium polyphosphate, grind 1.5 hours, prepare kaolin-barium sulfate-glycolic suspension, wherein kaolin-barium sulfate median size 0.36 μm.
5.0kg PTA is added in 20L typical zolymerization reactor, 3.0kgEG, 0.93g germanium dioxide, 413g above-mentioned kaolin-barium sulfate-second two suspension, 230 ~ 265 DEG C, carry out esterification under 0.2 ~ 0.3Mpa (gauge pressure), when aquifer yield reaches 1200ml, pressure release, to normal pressure, adds 0.44g trimethyl phosphite 99, atmospheric agitation 10 minutes, intensification degree of falling is pressed onto 280 DEG C and below 100Pa, reacts 1 ~ 3 hour.React complete and extrude through Melt Pump, pelletizing, drying, obtaining limiting viscosity is the sub-light polyester for film section of 0.610dl/g.
By obtained sub-light polyester for film section through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cool, make 70 μm of single thin films.Wherein extrusion temperature is 275 ~ 285 DEG C, and vertical La Wendu is 105 DEG C, and horizontal La Wendu is 105 DEG C, and vertical multiplying power of drawing is: 3.0: 1, and horizontal multiplying power of drawing is: 3.0: 1, setting temperature 180 DEG C, shaping time 1 second.
Embodiment 3
In sand mill, add 400ml granulated glass sphere, 300g kaolin, 100g barium sulfate, 400g ethylene glycol, 1.4g potassium polyphosphate, grind 1.5 hours, prepare kaolin-barium sulfate-glycolic suspension, wherein kaolin-barium sulfate median size 0.39 μm.
5.0kg PTA is added in 20L typical zolymerization reactor, 3.0kgEG, 1.71g antimony glycol, 402g above-mentioned kaolin-barium sulfate-second two suspension, 230 ~ 265 DEG C, carry out esterification under 0.2 ~ 0.3Mpa (gauge pressure), when aquifer yield reaches 1200ml, pressure release, to normal pressure, adds 0.84g triethyl phosphate, atmospheric agitation 10 minutes, intensification degree of falling is pressed onto 280 DEG C and below 100Pa, reacts 1 ~ 3 hour.React complete and extrude through Melt Pump, pelletizing, drying, obtaining limiting viscosity is the sub-light polyester for film section of 0.615dl/g.
By obtained sub-light polyester for film section through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cool, make 20 μm of single thin films.Wherein extrusion temperature is 275 ~ 285 DEG C, and vertical La Wendu is 110 DEG C, and horizontal La Wendu is 110 DEG C, and vertical multiplying power of drawing is: 3.6: 1, and horizontal multiplying power of drawing is: 3.6: 1, setting temperature 180 DEG C, shaping time 1 second.
Embodiment 4
Using sub-light polyester for film section obtained in embodiment 3 as two top layers, do not add the super bright PET chips of any additive as middle layer.Wherein two top layers account for 34% of film total amount, and middle layer accounts for 66% of film total amount.Cut into slices through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cool, make 20 μm of three-layer co-extruded films of ABA.Wherein extrusion temperature is 275 ~ 285 DEG C, and vertical La Wendu is 115 DEG C, and horizontal La Wendu is 115 DEG C, and vertical multiplying power of drawing is: 3.6: 1, and horizontal multiplying power of drawing is: 3.6: 1, setting temperature 180 DEG C, shaping time 1 second.
Reference example 1
In sand mill, add 400ml granulated glass sphere, 28g kaolin, 252g barium sulfate, 520g ethylene glycol, 0.7g potassium polyphosphate, grind 1.5 hours, prepare kaolin-barium sulfate-glycolic suspension, wherein kaolin-barium sulfate median size 0.36 μm.
5.0kg PTA is added in 20L typical zolymerization reactor, 3.0kgEG, 0.93g germanium dioxide, 413g above-mentioned kaolin-barium sulfate-second two suspension, 230 ~ 265 DEG C, carry out esterification under 0.2 ~ 0.3Mpa (gauge pressure), when aquifer yield reaches 1200ml, pressure release, to normal pressure, adds 0.44g trimethyl phosphite 99, atmospheric agitation 10 minutes, intensification degree of falling is pressed onto 280 DEG C and below 100Pa, reacts 1 ~ 3 hour.React complete and extrude through Melt Pump, pelletizing, drying, obtaining limiting viscosity is 0.615dl/g polyester slice.
By obtained polyester slice through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cooling, make 20 μm of single thin films.Wherein extrusion temperature is 275 ~ 285 DEG C, and vertical La Wendu is 110 DEG C, and horizontal La Wendu is 110 DEG C, and vertical multiplying power of drawing is: 3.6: 1, and horizontal multiplying power of drawing is: 3.6: 1, setting temperature 180 DEG C, shaping time 1 second.
Reference example 2
In sand mill, add 400ml granulated glass sphere, 280g barium sulfate, 520g ethylene glycol, 0.7g potassium polyphosphate, grind 1.5 hours, prepare kaolin-barium sulfate-glycolic suspension, wherein barium sulfate median size 0.35 μm.
5.0kg PTA is added in 20L typical zolymerization reactor, 3.0kgEG, 0.93g germanium dioxide, 413g above-mentioned barium sulfate-second two suspension, 230 ~ 265 DEG C, carry out esterification under 0.2 ~ 0.3Mpa (gauge pressure), when aquifer yield reaches 1200ml, pressure release, to normal pressure, adds 0.44g trimethyl phosphite 99, atmospheric agitation 10 minutes, intensification degree of falling is pressed onto 280 DEG C and below 100Pa, reacts 1 ~ 3 hour.React complete and extrude through Melt Pump, pelletizing, drying, obtaining limiting viscosity is 0.610dl/g polyester slice.
By obtained polyester slice through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cooling, make 20 μm of single thin films.Wherein extrusion temperature is 275 ~ 285 DEG C, and vertical La Wendu is 110 DEG C, and horizontal La Wendu is 110 DEG C, and vertical multiplying power of drawing is: 3.6: 1, and horizontal multiplying power of drawing is: 3.6: 1, setting temperature 180 DEG C, shaping time 1 second.
Reference example 3
By conventional do not add any additive superly have light polyester for film to cut into slices to cut into slices to mix according to certain proportioning with the conventional silicon dioxide polyester master batch that contains, in compound, dioxide-containing silica is 1000ppm, compound through pre-crystallized, dry, extrude, in length and breadth to two-way stretch, heat setting type, lax, cooling, make 70 μm of single thin films.Filming technology and embodiment one, two identical.
Reference example 4
The section of light polyester for film is had to prepare the three-layer co-extruded film of ABA with conventional cutting into slices containing silicon dioxide polyester master batch conventional the super of any additive of not adding.Wherein A layer is that the super silicon dioxide polyester master batch that contains having light polyester for film to cut into slices and to commonly use is cut into slices, and wherein dioxide-containing silica is 850ppm; The ratio that A layer accounts for total amount is 18% (mass ratio), and the ratio that B layer accounts for total amount is 82% (mass ratio).Each layer mixes according to above-mentioned proportioning, compound through pre-crystallized, dry, three-layer co-extruded go out, two-way stretch in length and breadth, heat setting type, lax, cooling, make 20 μm of three-layer co-extruded films.Filming technology is identical with embodiment four.
Table 1 embodiments of the invention and reference example film performance test result
Claims (10)
1. a preparation method for matt polyester film, is characterized in that: diprotic acid, dibasic alcohol, additive dispersion liquid are first carried out esterification under the effect of catalyzer, then adds stablizer and carry out polycondensation, obtains sub-light polyester for film; This sub-light polyester for film melt extrudes through super-dry, at 270 ~ 290 DEG C, and two-way stretch in length and breadth under temperature 80 ~ 120 DEG C, stretching ratio 3.0 ~ 4.0:1, heat setting type again, lax, cooling, traction, rolling, make the matt polyester film of single or multiple lift structure; Additive in described additive dispersion liquid is made up of mass content 60 ~ 80% kaolin and 40 ~ 20% barium sulfate, the median size of described additive is 0.3 ~ 0.5 μm, the dispersion solvent of described additive dispersion liquid is dibasic alcohol, and in described additive dispersion liquid, the consumption of additive is 1 ~ 5% of polyester quality.
2. method according to claim 1, is characterized in that: the thickness of described matt polyester film is 20 ~ 100 μm, and 45 degree of glossiness of this matt polyester film are less than 30%.
3. method according to claim 1, is characterized in that: described diprotic acid is PTA or QTA, and described dibasic alcohol is ethylene glycol; Described diprotic acid is 1:1.2 ~ 1:2.0 with the ratio of the molar weight of ethylene glycol.
4. method according to claim 1 and 2, is characterized in that: the mass concentration of described additive dispersion liquid is 20 ~ 60%.
5. method according to claim 1, is characterized in that: the dispersion agent also containing additive quality 0.1 ~ 0.5% in described additive dispersion liquid, described dispersion agent is sodium polyphosphate or potassium polyphosphate.
6. method according to claim 1, is characterized in that: described catalyzer is germanium, antimony or titanium class catalyzer, and the consumption of catalyzer is 0.01 ~ 0.09% of polyester quality.
7. method according to claim 1, is characterized in that: described stablizer is phosphoric acid, phosphorous acid, Tripyrophosphoric acid, trimethyl phosphite 99, triphenylphosphate or triethyl phosphate, and the consumption of described stablizer is 0.0003 ~ 0.040% of polyester quality.
8. method according to claim 1, is characterized in that: the temperature of described esterification is 210 ~ 280 DEG C, and absolute pressure is 0.1 ~ 0.5MPa; The temperature of described polycondensation is 250 ~ 295 DEG C, polycondensation absolute pressure≤1KPa, and the reaction times is 0.5 ~ 4 hour.
9. method according to claim 1, is characterized in that: the temperature of described heat setting type is 180 DEG C-230 DEG C, and shaping time is 1 ~ 3 second.
10. method according to claim 1, is characterized in that: the limiting viscosity of described sub-light polyester for film is 0. 55 ~ 0.70dl/g.
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| CN201110353645.XA CN103102474B (en) | 2011-11-09 | 2011-11-09 | Matt polyester film preparation method |
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| CN201110353645.XA CN103102474B (en) | 2011-11-09 | 2011-11-09 | Matt polyester film preparation method |
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| CN103102474B true CN103102474B (en) | 2015-01-14 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105415722A (en) * | 2015-11-23 | 2016-03-23 | 安徽国泰印务有限公司 | Preparation process for matte aluminized polyester film |
| CN109130422B (en) * | 2018-07-12 | 2020-11-03 | 浙江和顺新材料有限公司 | Matte biaxially oriented polyester film and preparation method thereof |
| CN114685766B (en) * | 2020-12-31 | 2024-02-02 | 中国石油化工股份有限公司 | Modified biodegradable polyester and preparation method thereof |
| CN113801442B (en) * | 2021-09-17 | 2022-12-13 | 浙江强盟实业股份有限公司 | Low-shrinkage matte polyester film master batch, polyester film and preparation method of polyester film |
| CN114702789B (en) * | 2022-03-01 | 2023-12-19 | 杭州和顺科技股份有限公司 | High-light-transmittance polyester film and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1230566A (en) * | 1998-03-30 | 1999-10-06 | 平湖塑料厂 | Glazed plastic film for liquid packing |
| CN1826373A (en) * | 2003-07-03 | 2006-08-30 | 罗狄亚特性纤维公司 | Mineral fillers for enhancing opacity of thermoplastic polymers |
| CN101333329A (en) * | 2008-08-06 | 2008-12-31 | 中国石化仪征化纤股份有限公司 | Method for making polyester for low-haze biaxial stretching polyester film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1230566A (en) * | 1998-03-30 | 1999-10-06 | 平湖塑料厂 | Glazed plastic film for liquid packing |
| CN1826373A (en) * | 2003-07-03 | 2006-08-30 | 罗狄亚特性纤维公司 | Mineral fillers for enhancing opacity of thermoplastic polymers |
| CN101333329A (en) * | 2008-08-06 | 2008-12-31 | 中国石化仪征化纤股份有限公司 | Method for making polyester for low-haze biaxial stretching polyester film |
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