CN102241177A - Colorful polyester film and preparation method thereof - Google Patents
Colorful polyester film and preparation method thereof Download PDFInfo
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- CN102241177A CN102241177A CN2011100767344A CN201110076734A CN102241177A CN 102241177 A CN102241177 A CN 102241177A CN 2011100767344 A CN2011100767344 A CN 2011100767344A CN 201110076734 A CN201110076734 A CN 201110076734A CN 102241177 A CN102241177 A CN 102241177A
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Abstract
The invention discloses a colorful polyester film and a preparation method thereof. The colorful polyester film comprises at least a polyester layer containing pigment and at least a polyester layer without pigment, wherein two external surfaces of the colorful polyester film are not both polyester layers containing pigment at the same time. The polyester layer without pigment comprises components of, by weight, 300ppm-800ppm of inorganic additive, with the balance of modified polyester. The polyester layer containing pigment comprises components of, by weight, 92%-99.99% of modified polyester, 0.001%-3% of dispersant, 0.01%-5% of pigment or dye and 300ppm-800ppm of inorganic additive. Raw materials of the invention are easily available, and a preparation technology is simple and scientific, and overcomes many disadvantages of a prior art, so that when the colorful polyester film contacts with food, pigment or additive will not migrate into the food. Therefore, the colorful polyester film is safe, healthy and energy saving, has strong color endurance and good adhesiveness to metal, and can satisfy demands of internal and external packings of foodstuff and beverage cans.
Description
Technical field
The present invention relates to thin film technique, relate in particular to a kind of color polyester film and preparation method thereof.
Background technology
In the mental package industry, can contents such as drink and food are because the color of self and have color to require (making beverage or food seem more can transfer consumer's appetite) to metal can inwall applicator, and existing common color polyester film can't satisfy the safe and sanitary, color stability of liquid state, fluid food and to the performance demands such as applying of metal.
At present, domestic main employing coating coating metal jar inwall, and it is hard and crisp behind the paint solidification, ductility, the impact resistance of coating are relatively poor, can not carry out the bigger processing and forming of deformation with the metallic plate after its coating, therefore the bigger seamless tin of deformation sprays the technology relative complex usually to material behind jug forming.In addition, though the paint metal jar has certain corrosion resistance, but in the process of paint solidification, need to evaporate a large amount of solvents, to in 180~220 ℃ baking oven, toast 10~20 minutes, this not only needs to consume a large amount of energy, and organic solvent may be brought in the air and contaminated environment also will cause actual bodily harm to the operator.
Patent CN 1126139A has introduced a kind of thin metal layer polyester film that is used for, and this film adopts the titanium oxide that adds more than 10%, obtains the polyester film of complete shading.But the pigment dispersion force is poor in this type of film, and effectively the dispersed color molecule prepares the color polyester film of low pigment content, needs to add a large amount of pigment (quality percentage composition 10~30%) and could satisfy white requirement uniformly; And all contain titanium dioxide in the thin layer, can cause bigger pollution, increased the cleaning difficulty film production equipment.
Patent CN 1284913A (E.I.Du Pont Company) has introduced a kind of polyester film and preparation method of low pigment content, its pigment is titanium dioxide, because the main purpose of this its invention of film is in order to prepare the high film of opacity, typical content has also reached 10wt%, does not almost have light transmission.In addition, this preparation scheme effectively the dispersed color molecule prepare the polyester film of low pigment content and organic pigment.
Patent JP-A-8290539 (Diafoil Hoechst company) discloses a kind of film that is suitable as magnetic recording medium.Film internal layer comprises the fluorescent fine particles and the outer polyester film that comprises Chinese white in this patent, and film contains two different additive layers.This and, its purpose of design of such film mainly is in order to satisfy the application of magnetic recording medium aspect, not possess the good fit to metal.
Patent CN 101195685A has introduced a kind of full-dull colorful insulation polyester film and production technology thereof; this film adopts matt film grade polyester chip, colored Masterbatch and contains silica polyester master particle combination drying extrudes preparation single structure polyester film, to satisfy the application in electronics, wire rod, insulation such as electric.But the film two sides all has pigment meeting severe contamination plant equipment in this patent, causes the defective of cleaning difficulty and reducing the film production usage ratio of equipment.Even improved production cost, can not satisfy the packaging for foodstuff field, particularly flexible package punch field that have pigment migration to require to the surface; In addition, this film adopts conventional polyester, the applying metal that can not be fit to; Used a large amount of silica dioxide delustring agents in the film, the film surface glossiness is low.
To sum up, existing film all can not satisfy the heat posted metallic plate, effectively stop pigment migration in food, and keeps the needs of the durability of film color gloss.Ubiquity, the shortcoming that the pigment demand is big, contain poisonous and harmful substance, production cost height, production technology and equipment complexity, film and metal-clad weak effect.
Summary of the invention
The invention provides a kind of color polyester film, in order to solve defective of the prior art, implementation structure is simple, raw material is easily got and is easy to get, can not take place that pigment and additive are moved in the food, safety and sanitation are energy-conservation, color durability height, good to metal-clad when the Food Contact, satisfies food, beverage metal can exterior and interior packing demand.
A kind of color polyester film comprises: one deck contains the polyester layer of pigment and the unpigmented polyester layer of one deck at least at least, and two outer surfaces of color polyester film are simultaneously for containing the polyester layer of pigment.
Described unpigmented polyester layer comprises each component that weight ratio is following: the anti-stick inorganic additive 300ppm~800ppm that connects, and surplus is a modified poly ester;
The described polyester layer that contains pigment comprises each component that weight ratio is following:
Modified poly ester 92%~99.99%;
Dispersant 0.01 ‰~3%;
Pigment or dyestuff 0.1 ‰~5%;
The anti-stick inorganic additive 300ppm~800ppm that connects.
Further, described unpigmented polyester layer comprises each component that weight ratio is following: the anti-stick inorganic additive 300ppm~800ppm that connects, and surplus is a modified poly ester;
The described polyester layer that contains pigment comprises each component that weight ratio is following:
Modified poly ester 95%~99.99%;
Dispersant 0.01 ‰~2%;
Pigment or dyestuff 0.1 ‰~3%;
The anti-stick inorganic additive 300ppm~800ppm that connects.
Further, described dispersant is an organic dispersing agent.Described organic dispersing agent is a polyolefin.Described organic dispersing agent is one or more in polyethylene, oxidic polyethylene, polypropylene, white oil and the silicone oil.
Further, described modified poly ester adopts binary acid (as: terephthalic acid (TPA), M-phthalic acid, adipic acid, decanedioic acid etc.) with polyalcohol (as ethylene glycol, propane diols, butanediol, diglycol, neopentyl glycol, 1.4-cyclohexanedimethanol, trimethylolpropane etc.) through esterification, polycondensation and make mylar is specially the PETG of isophthalate modified, the PETG of butanediol ester modification, the PETG of propylene glycol ester modification, cyclohexane is in the ester modified PETG of dimethanol one or more.
Further, the molar content of modified monomer is 0.01%~30% in the described modified poly ester.Modified monomer in the described modified poly ester is M-phthalic acid, propane diols, butanediol and cyclohexane in the dimethanol one or more.
Further, described anti-stick even inorganic additive is SiO
2, CaCO
3With in the talcum powder one or more.
Further, described pigment or dyestuff both can be that inorganic matter also can be an organic matter, especially met pigment or dyestuff in GB-9685 food containers, the packaging material used additives use sanitary standard.
The present invention also provides the preparation method of described color polyester film simultaneously, to realize that preparation method's science, equipment are simple, high efficiency, can obtain rerum natura and all good color polyester films of form.
The preparation method of color polyester film comprises the steps:
(1) component and the described component that contains the polyester layer of pigment of described unpigmented polyester layer are mixed respectively, dry, extruded, casts sheet by extruder;
(2) described casting sheet is through longitudinal stretching, cross directional stretch film forming, the film thermal finalization after will stretching then;
(3) film after the thermal finalization cool off, rolling and cutting.
Further, dry described in the step (1) and on ebullated bed, finish, 120 ℃~170 ℃ of bake out temperatures, drying time is no less than 4 hours.
Further, described extrusion temperature is 230 ℃~285 ℃.
Further, described casting sheet thickness should be controlled at 0.1mm~2mm, and the thickness that can make polyester film is at 10 μ m~60 μ m.
Further, described longitudinal stretching preheat temperature is 80 ℃~160 ℃, and described cross directional stretch preheat temperature is 90 ℃~140 ℃, and draw ratio is 2.0~4.8.
Further, described heat setting temperature is 150 ℃~225 ℃, heat-setting time 6S~18S.
But the coating such as phenolic aldehyde epoxy on the present invention's substituted metal jar packing inner surface.A kind of metal can packing, described color polyester film heat posted is on metal, and described color polyester film is unpigmented polyester layer away from a side of metal.
Color polyester film raw material of the present invention is easily got and is easy to get, and the simple science of preparation method mainly has following several respects advantage compared with prior art:
(1) described color polyester film and beverage, Food Contact layer do not contain pigment or dyestuff, keep more stable with respect to other toning mode pigment or dyestuff, can not move in the food, and the color durability is higher, more environmentally-friendly sanitary health;
(2) described color polyester film outer surface or two outer surfaces do not contain additives of pigments, have reduced the pollution to plant equipment of melt resin and film, have reduced the workload and the time of artificial cleaning, have improved the service efficiency of machine;
(3) described color polyester film color uniformity height,, good with crowd product aberration Lab value Δ E to metal-clad less than 0.3, satisfy food, beverage metal can exterior and interior packing demand.For there is color demand mental package paint replacement material in a new generation.
The specific embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the invention, the technical scheme in the embodiment of the invention is clearly and completely described, obviously, described embodiment is the present invention's part embodiment, rather than whole embodiment.Based on the embodiment among the present invention, those of ordinary skills belong to the scope of protection of the invention not making the every other embodiment that is obtained under the creative work prerequisite.
A kind of color polyester film comprises: one deck contains the polyester layer of pigment and the unpigmented polyester layer of one deck at least at least, and two outer surfaces of color polyester film are simultaneously for containing the polyester layer of pigment.
Unpigmented polyester layer comprises each component that weight ratio is following: the anti-stick inorganic additive 300ppm~800ppm that connects, and surplus is a modified poly ester;
The polyester layer that contains pigment comprises each component that weight ratio is following:
Modified poly ester 92%~99.99%;
Dispersant 0.01 ‰~3%;
Pigment or dyestuff 0.1 ‰~5%;
The anti-stick inorganic additive 300ppm~800ppm that connects.
The preparation method that the preparation of color polyester film promptly can be adopted conventional plural layers, also can adopt following method:
(1) unpigmented polyester layer component and the polyester layer component that contains pigment mixed respectively, dries, is cooled to the casting sheet after extruding, be adhesive into one by screw extruder; Wherein the interpolation of raw material order and mixed method do not influence the present invention, for example contain the preparation of the polyester of pigment, both can have each component directly to mix, dry and obtain; After also can in the unpigmented polyester for preparing, adding pigment or dyestuff, dispersant, mix again, dry and obtain.
(2) cast sheet through longitudinal stretching, cross directional stretch film forming, the film thermal finalization after will stretching then;
(3) film after the thermal finalization cool off, rolling and cutting.
Embodiment 1
Unpigmented polyester layer comprises each component that weight ratio is following: 400ppm SiO
2Powder, all the other are the PETG of isophthalate modified (wherein the molar content of M-phthalic acid is 15%);
The polyester layer that contains pigment comprises each component that weight ratio is following:
The PETG of isophthalate modified (wherein the content mol ratio of M-phthalic acid is 15%) 97%;
Polyolefin 1%;
Pigment yellow 147 2%;
SiO
2Powder 400ppm.
After testing, the fusing point of the PETG of isophthalate modified is 210 ℃~240 ℃, and glass transition temperature is at 60 ℃~80 ℃.According to above proportioning each component is mixed with out unpigmented polyester and the polyester that contains pigment, then they is being dried 130 ℃ of bake out temperatures, drying time 4 hours on ebullated bed.Wherein also can make the polyester that contains pigment through mixing, drying by in unpigmented polyester, adding pigment and dispersant.
The preparation method of color polyester film: the unpigmented polyester after will drying is extruded through the extruder that A layer die orifice links to each other; The polyester that will contain pigment is extruded through the extruder of B layer die orifice, extruding dies is a two-layer mouthful of mould, unpigmented polyester is sticked together at the extruder mouth with the polyester that contains pigment, form behind the chilling and have double-decker color polyester film casting sheet, each section of extruder screw heating-up temperature is 245 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃ (from spouts to a mouthful mould direction), the extruder screw rotating speed is 100 commentaries on classics/min, and casting sheet thickness is 0.20mm.Casting sheet longitudinal stretching at first, it is vertical that to draw preheat temperature be 80 ℃, draw ratio 2.5, cross directional stretch then, the horizontal preheat temperature of drawing is 120 ℃, draw ratio 3.4.Film after the stretching is 200 ℃ of thermal finalizations, heat-setting time 10S, and last film cools off, rolling and cutting.As shown in table 1 by the color polyester film performance test that said method makes
Table 1 embodiment 1 color polyester film performance test
Embodiment 2
Unpigmented polyester layer comprises each component that weight ratio is following: SiO
2Powder 500ppm, all the other are the PETG of isophthalate modified (wherein the molar content of M-phthalic acid is 15%);
The polyester layer that contains pigment comprises each component that weight ratio is following:
The PETG of isophthalate modified (wherein the content mol ratio of M-phthalic acid is 15%) 98.7%;
Polyolefin-wax 0.3%;
Pigment yellow 13 8 1%;
SiO
2Powder 500ppm;
After testing, the fusing point of the PETG of isophthalate modified is 210 ℃~240 ℃, and glass transition temperature is at 60 ℃~80 ℃.According to above proportioning each component is mixed with out unpigmented polyester and the polyester that contains pigment, then they is being dried 130 ℃ of bake out temperatures, drying time 4 hours on ebullated bed.Wherein also can make the polyester that contains pigment through mixing, drying by in unpigmented polyester, adding pigment and dispersant.
The preparation method of color polyester film: the unpigmented polyester after will drying is extruded with the extruder that B layer die orifice links to each other through the A layer; The polyester that will contain pigment is extruded through the extruder of C layer die orifice, extruding dies is three layers of mouth mould, unpigmented polyester is sticked together at the extruder mouth with the polyester that contains pigment, form behind the chilling and have three-decker color polyester film casting sheet, each section of extruder screw heating-up temperature is 245 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃ (from spouts to a mouthful mould direction), the extruder screw rotating speed is 100 commentaries on classics/min, and casting sheet thickness is 0.2mm.Casting sheet longitudinal stretching at first, it is vertical that to draw preheat temperature be 80 ℃, draw ratio 2.8, cross directional stretch then, the horizontal preheat temperature of drawing is 110 ℃, draw ratio 3.6.Film after the stretching is 200 ℃ of thermal finalizations, heat-setting time 8S, and last film cools off, rolling and cutting.As shown in table 2 by the color polyester film performance test that said method makes.
Table 2 embodiment 2 color polyester film performance tests:
Embodiment 3
Unpigmented polyester layer comprises each component that weight ratio is following: 700ppm CaCO
3Powder, all the other are the PETG of ethylene isophthalate modification (wherein the molar content of M-phthalic acid is 3%);
The polyester layer that contains pigment comprises each component that weight ratio is following:
The PETG of ethylene isophthalate modification (wherein the content mol ratio of M-phthalic acid is 3%) 99.5%;
Polyolefin-wax 0.1%;
Pigment red 21 4 0.4%;
CaCO
3Powder 700ppm;
After testing, the fusing point of the PETG of ethylene isophthalate modification is 230 ℃~260 ℃, and glass transition temperature is at 60 ℃~80 ℃.According to above prescription each component is mixed with out unpigmented polyester and the polyester that contains pigment, then they is being dried 140 ℃ of bake out temperatures, drying time 4 hours on ebullated bed.Wherein also can make the polyester that contains pigment through mixing, drying by in unpigmented polyester, adding pigment and dispersant.
The preparation method of color polyester film: the unpigmented polyester after will drying is extruded through the extruder that the A layer links to each other; The polyester that will contain pigment is extruded through the extruder of B layer and C layer die orifice, extruding dies is three layers of mouth mould, unpigmented polyester is sticked together at the extruder mouth with the polyester that contains pigment, form behind the chilling and have three-decker color polyester film casting sheet, each section of extruder screw heating-up temperature is 120 ℃, 255 ℃, 265 ℃, 275 ℃, 280 ℃ (from spouts to a mouthful mould direction), the extruder screw rotating speed is 100 commentaries on classics/min, and casting sheet thickness is 0.2mm.Casting sheet longitudinal stretching at first, it is vertical that to draw preheat temperature be 80 ℃, draw ratio 3.2, cross directional stretch then, the horizontal preheat temperature of drawing is 120 ℃, draw ratio 3.6.Film after the stretching is 210 ℃ of thermal finalizations, heat-setting time 8S, and last film cools off, rolling and cutting.As shown in table 3 by the color polyester film performance test that said method makes
Table 3 embodiment 3 color polyester film performance tests:
Embodiment 4
Unpigmented polyester layer comprises each component that weight ratio is following: 400ppm CaCO
3Powder, all the other are the PETG of isophthalate modified (wherein the molar content of M-phthalic acid is 10%);
The polyester layer that contains pigment comprises each component that weight ratio is following:
The PETG of isophthalate modified (wherein the molar content of M-phthalic acid is 10%) 97.5%;
Polyolefin-wax 0.1%;
Pigment yellow 042 1.5%;
CaCO
3Powder 400ppm;
After testing, the fusing point of the PETG of isophthalate modified is 200 ℃~240 ℃, and glass transition temperature is at 60 ℃~80 ℃.According to above proportioning each component is mixed with out unpigmented polyester and the polyester that contains pigment, then they is being dried 120 ℃ of bake out temperatures, drying time 4 hours on ebullated bed.Wherein also can make the polyester that contains pigment through mixing, drying by in unpigmented polyester, adding pigment and dispersant.
The preparation method of color polyester film: unpigmented polyester is extruded with the extruder that C layer die orifice links to each other through the A layer; The polyester that will contain pigment is extruded through the extruder of B layer die orifice, the extruder mouth is three layers of mouth mould, unpigmented polyester is sticked together at the extruder mouth with the polyester that contains pigment, form behind the chilling and have three-decker color polyester film casting sheet, be to be coated with one deck in the two-layer unpigmented polyester to contain the pigment polyester, each section of extruder screw heating-up temperature is 245 ℃, 255 ℃, 260 ℃, 265 ℃, 270 ℃ (from spouts to a mouthful mould direction), the extruder screw rotating speed is 100 commentaries on classics/min, and casting sheet thickness is 0.2mm.Casting sheet longitudinal stretching at first, it is vertical that to draw preheat temperature be 80 ℃, draw ratio 3.5, cross directional stretch then, the horizontal preheat temperature of drawing is 110 ℃, draw ratio 4.6.Film after the stretching is 200 ℃ of thermal finalizations, heat-setting time 8S, and last film cools off, rolling and cutting.As shown in table 4 by the color polyester film performance test that said method makes
Table 4 embodiment 4 color polyester film performance tests:
The color polyester film for preparing among above-mentioned 1~4 embodiment is attached on the metal, makes the metal can packing, preparation method is as follows:
The polyester film that embodiment 1~4 is prepared under 240 ℃, 6Kg pressure respectively heat fit on the thick metal substrate of 0.20mm (thin steel of chromium plating and the thin aluminum sheet) surface, be washed into the cup-shaped sample (precoated steel sheet and drift are not coated with lubricating oil) of diameter 30mm, dark 8mm with dashing will the fit metal substrate of polyester film of cup experimental machine.
The overlay film iron that adopts the present invention's preparation in impact process, do not have between film and the metal substrate separate, unsticking.Should place 121 ℃ of distilled water boiling 30min by cup-shaped sample, the prepared polyester film surface of embodiment 1~4 is wrinkle resistant, with between the metal substrate do not separate, aberration Δ E is less than 0.3 before and after the boiling, should place 121 ℃ by cup-shaped sample, mass concentration is boiling 30min in 3% citric acid solution, four kinds of film surfaces are all wrinkle resistant, with between the metal substrate do not separate, and aberration Δ E is less than 0.5.
Same, in taggers tin, through dashing cup, poach and 121 ℃ of 3% acetum boilings down, film has all showed good performance with heat posted under the same condition of the film of embodiment 1-4, and experimental result is with the same on chrome plating or aluminium sheet.
Hydrochloric acid solution or pH ≈ 11 sodium hydroxide lyes of the pH ≈ 3 that embodiment 1~4 color polyester film is put into soak, and the color change Δ Lab value Δ E of film is as shown in table 5:
The color change test of table 5 embodiment 5 color polyester films
More than implement to illustrate that color polyester film provided by the present invention can be fitted in metal substrate (sheet metal and thin aluminum sheet) surface, be fit to following process such as system jar, colour-fast in the acid ﹠ alkali liquid digestion process, color stability is good, and the Δ Lab value Δ E of batch product is less than 0.3 together, COLOR COMPOSITION THROUGH DISTRIBUTION is even, is to solve the effective ways of packing content things such as beverage can, food cans to the demand of color.
It should be noted that at last: above embodiment only in order to technical scheme of the present invention to be described, is not intended to limit; Although with reference to previous embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that: it still can be made amendment to the technical scheme that aforementioned each embodiment put down in writing, and perhaps part technical characterictic wherein is equal to replacement; And these modifications or replacement do not make the essence of appropriate technical solution break away from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (11)
1. a color polyester film is characterized in that, comprising: one deck contains the polyester layer of pigment and the unpigmented polyester layer of one deck at least at least, and two outer surfaces of color polyester film are simultaneously for containing the polyester layer of pigment;
Described unpigmented polyester layer comprises each component that weight ratio is following: the anti-stick inorganic additive 300ppm~800ppm that connects, and surplus is a modified poly ester;
The described polyester layer that contains pigment comprises each component that weight ratio is following:
Modified poly ester 92%~99.99%;
Dispersant 0.01 ‰~3%;
Pigment or dyestuff 0.1 ‰~5%;
The anti-stick inorganic additive 300ppm~800ppm that connects.
2. color polyester film according to claim 1 is characterized in that, described unpigmented polyester layer comprises each component that weight ratio is following: the anti-stick inorganic additive 300ppm~800ppm that connects, and surplus is a modified poly ester;
The described polyester layer that contains pigment comprises each component that weight ratio is following:
Modified poly ester 95%~99.99%;
Dispersant 0.01 ‰~2%;
Pigment or dyestuff 0.1 ‰~3%;
The anti-stick inorganic additive 300ppm~800ppm that connects.
3. color polyester film according to claim 1 and 2 is characterized in that, described dispersant is an organic dispersing agent, and described organic dispersing agent is one or more in polyethylene, oxidic polyethylene, polypropylene, white oil and the silicone oil.
4. color polyester film according to claim 1 and 2, it is characterized in that described modified poly ester is that the PETG, cyclohexane of PETG, the propylene glycol ester modification of PETG, the butanediol ester modification of isophthalate modified is in the ester modified PETG of dimethanol one or more.
5. color polyester film according to claim 1 and 2 is characterized in that, the molar content of modified monomer is 0.01%~30% in the described modified poly ester.
6. color polyester film according to claim 1 and 2 is characterized in that, described anti-stick even inorganic additive is SiO
2, CaCO
3With in the talcum powder one or more.
7. the preparation method of the arbitrary described color polyester film of claim 1~6 is characterized in that, comprises the steps:
(1) described unpigmented polyester layer component and the described polyester layer component that contains pigment mixed respectively, dries, is cooled to the casting sheet after extruding, be adhesive into one by screw extruder;
(2) described casting sheet is through longitudinal stretching, cross directional stretch film forming, the film thermal finalization after will stretching then;
(3) film after the thermal finalization cool off, rolling and cutting.
8. the preparation method of color polyester film according to claim 7 is characterized in that, dry described in the step (1) and on ebullated bed, finish, and 120 ℃~170 ℃ of bake out temperatures, drying time is no less than 4 hours.
9. the preparation method of color polyester film according to claim 7 is characterized in that, described casting sheet THICKNESS CONTROL is at 0.1mm~2mm.
10. the preparation method of color polyester film according to claim 7 is characterized in that, described longitudinal stretching preheat temperature is 80 ℃~160 ℃, and described cross directional stretch preheat temperature is 90 ℃~220 ℃, and draw ratio is 2.0~4.8.
11. the preparation method of color polyester film according to claim 7 is characterized in that, described heat setting temperature is 150 ℃~225 ℃, heat-setting time 6S~18S.
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Application publication date: 20111116 |