CN101293412A - Special optical level polyester film and production method thereof - Google Patents
Special optical level polyester film and production method thereof Download PDFInfo
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- CN101293412A CN101293412A CNA2008101240492A CN200810124049A CN101293412A CN 101293412 A CN101293412 A CN 101293412A CN A2008101240492 A CNA2008101240492 A CN A2008101240492A CN 200810124049 A CN200810124049 A CN 200810124049A CN 101293412 A CN101293412 A CN 101293412A
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Abstract
The invention relates to the manufacture field of a plastic film, in particular to a polyester film which has special requirements on optical property and a preparation method thereof; the invention solves the defects on the property aspects such as the transparency, the lustrousness and the haze of the film caused by the defects on the aspects such as the raw materials, the manufacture technique and the manufacture technique condition control of the existing polyester film. The polyester film is manufactured by three-layer co-extrusion, bidirectional stretching and corona processing; the three layers after the co-extrusion and the stretching are two surface layers and an intermediate layer; the intermediate layer is the polyester layer containing 0 to 25 percent of a polyester feed back and a polyester polymer as the rest amount according to the weight proportion; the two surface layers are the polyester layer containing 300 to 1500ppm of an antiblocking agent silicon dioxide and a polyester polymer as the rest amount according to the weight proportion; the polyester polymer includes 8.0 to 9.0:1:5.0 to 5.5 of phthalic acid, m-phthalic acid and glycol according to the weight proportion; the thickness of the surface layers accounts for 5 to 15 percent of the total thickness of the whole film and the thickness of the intermediate layer accounts for 70 to 90 percent of the total thickness of the whole film.
Description
Technical field
The present invention relates to plastic sheeting and make the field, especially a kind of polyester film of optical property being had specific (special) requirements and preparation method thereof that is used for, as: automobile and glass for building purposes pad pasting, LCD with polyester film, high-grade minute surface aluminium plating basement membrane and highway communication facility with reflective membrane etc.
Background technology
The optical property of existing polyester film, as transparency, aspect of performance such as glossiness and mist degree exists not enough, its main cause is because the raw-material selection of polyester film, there are defective in the optimization of technical recipe and the multinomial technical measures such as regulation and control of manufacturing condition, more concrete reason is: one, the raw material aspect, one of primary raw material of polyester film is mylar section (being called for short the PET section), it is a kind of crystalline polymer, it is to be that polycondensation forms under the condition of certain technological temperature and vacuum under the effect of catalyst at antimony oxide by terephthalic acid (TPA) and ethylene glycol.Because of its in film forming procedure, can produce certain degree of crystallinity, so have influence on the optical property of film; Another important raw and processed materials of polyester film is an antiblocking agent, because polyester film batches and cuts in two operations production process, in order to prevent that generation is inter-adhesive between the film, and the use that unreels that makes things convenient for downstream user, must add a certain proportion of antiblocking agent when film production, the kind of antiblocking agent is a lot, and model is different, refraction index and polyester also there are differences, and the improper use of antiblocking agent has also influenced the optical of film; Two, production technology aspect, the old production technology of polyester film is that individual layer is extruded, be that a single screw extrusion machine is adopted in melt extruding of polyester slice, complicated pre-crystallizing and drying system is equipped with and, for solving the anti-adhesion problem of film, the amount of the employed antiblocking agent of single-layer PET film is just many, and the antiblocking agent consumption is many more, and is also just big more to the Film Optics Effect on Performance; Three, in manufacturing condition control, improper to the structure control of technological temperature, crystalline rate and crystallite, also influenced the optical property of film.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of polyester film of optical property being had specific (special) requirements and preparation method thereof that is used for is provided, overcomes existing polyester film because the deficiency of the aspect of performances such as the film clarity that defective caused, glossiness and mist degree of raw material aspect, production technology aspect and manufacturing condition control aspect.
The technical solution adopted for the present invention to solve the technical problems is: special optical level polyester film, described polyester film is made through three-layer co-extruded and biaxial tension, sided corona treatment, the non-common homopolymers of the polyester that is adopted, but employing terpolymer resin, purpose is the crystal property of partial destruction polyester, adopting three-layer co-extruded is in order to reduce the consumption of antiblocking agent, thereby reduces the influence of antiblocking agent to optical property; Three layers after co-extrusion stretches is two superficial layers and intermediate layer; Described intermediate layer is the polyester layer that contains the polyester polymers of the polyester feed back of weight ratio 0～25% and surplus, and described two superficial layers all are the polyester layer that contains the polyester polymers of the antiblocking agent silica of weight ratio 300～1500ppm and surplus; Described polyester polymers comprises weight ratio 8.0～9.0: 1: 5.0～5.5 phthalic acid, M-phthalic acid and ethylene glycol; Described antiblocking agent silica is micron order antiblocking agent silica; Described two superficial layers respectively account for 5～15% of overall film thickness, and the thickness in intermediate layer accounts for 70～90% of total overall film thickness.
The preparation method of above-mentioned special optical level polyester film has the process of being prepared as follows:
(a) preparation process of polyester slice, phthalic acid and M-phthalic acid are made mixture by weight 8.0～9.0: 1 ratio, again aforesaid mixture is added in the making beating still by weight 1: 0.50～0.55 with ethylene glycol, the phosphoric acid ester stabilizing agent that adds aforesaid mixture and ethylene glycol gross weight 0.03～0.04% simultaneously, the antimony oxide catalyst of aforesaid mixture and ethylene glycol gross weight 0.03～0.04%, in the making beating still, pulled an oar 30～40 minutes, import esterifying kettle then and carry out esterification, temperature control is at 220～250 ℃ in the esterification, 170～180 ℃ of fractionation column temperatures, reaction time of esterification 0.1～5 hour, then, carry out polycondensation reaction at 260～290 ℃, discharging underwater cutpellet after polycondensation reaction is finished through filtering the importing polycondensation vessel, the air-dry polyester slice of making;
(b) batch mixes, crystallizing and drying process are prepared first, second surface layer raw material of two superficial layers and intermediate layer raw material respectively, the intermediate layer raw material be the polyester slice made in the process (a) and with the polyester feed back of polyester slice weight ratio 0～25%; First, second surface layer raw material is made up of polyester slice of making in the process (a) and micron order antiblocking agent silica, and the weight ratio content of described silica in raw material is 300～1500PPm; Also will give crystallization and drying to the intermediate layer raw material, giving crystallization and baking temperature is 150～170 ℃, and 3.5～4 hours time, dried intermediate layer raw material moisture content is less than 40ppm;
(c) melt extrude casting sheet process, ready raw material in the process (b) is invested extruder, extrude the continuous casting sheet with three-decker of one through the co-extrusion die head of extruder, extrusion temperature is controlled at 280～285 ℃, and the chilling temperature of Quench drum is controlled at below 40 ℃;
(d) longitudinal stretching process, on longitudinal stretching machine, the casting sheet is carried out twice longitudinal stretching continuously, draw ratio is 1.5～2.0: 1 for the first time, draw ratio is 2.2～3.0: 1 for the second time, the casting sheet place of being stretched heating-up temperature is 120～130 ℃ during longitudinal stretching, behind the longitudinal stretching film is carried out cooling and shaping and handle 20～30 ℃ of chilling temperatures;
(e) cross directional stretch process, on the cross directional stretch machine film after the longitudinal stretching process is being carried out cross directional stretch, cross directional stretch multiplying power 3.2～4.2: 1, the film place of being stretched temperature is 110～130 ℃ during cross directional stretch, the casting sheet place of being stretched carries out The pre-heat treatment before the cross directional stretch, 60～105 ℃ of preheat temperatures, 1～3 second preheating time, behind the cross directional stretch film is carried out thermal finalization and loose cooling processing, 190～230 ℃ of heat setting temperatures, heat-setting time 2～5 seconds, 80～120 ℃ of lax chilling temperatures;
(f) sided corona treatment process is carried out the single or double sided corona treatment to film, to increase surface tension;
(g) traction wrapup procedure, film carries out rolling under the traction of carry-over pinch rolls.
The invention has the beneficial effects as follows, superior performances such as polyester film transparency of the present invention, glossiness and mist degree, reason is: the first, aspect raw material owing to adopt the 3rd monomer---M-phthalic acid partly replaces terephthalic acid (TPA) to participate in copolycondensation, weakening, degree of crystallinity that the mylar crystal property that is generated is subjected to a certain degree decrease, thereby the optical property of film is increased; The second, remain and selected the refraction index silica close with polyester to do the antiblocking agent of film aspect raw material, thereby both solved the anti-adhesion problem of film, reaching does not again influence or the purpose of little effect Film Optics performance; The 3rd, aspect production technology, the old production technology of polyester film is that individual layer is extruded, be that a single screw extrusion machine is adopted in melt extruding of polyester slice, complicated pre-crystallizing and drying system is equipped with and, for solving the anti-adhesion problem of film, the amount of the employed antiblocking agent of single-layer polyester film is just many, the antiblocking agent consumption is many more, also just big more to the Film Optics Effect on Performance, the present invention adopts the polyester film of the multi-layer co-extruded process route of three extruders with the production three-decker, wherein, two superficial layer first surface layers, each only accounts for about 5～15% of whole film thickness second surface thickness, the intermediate layer then accounts for 70～90%, so only needing to add an amount of antiblocking agent at superficial layer gets final product, with 12 microns polyester films is example, single-layer polyester film in this way, generally need add the about 1200PPM*12=14400ppm of antiblocking agent, if change three-decker into, only need to add 1200*2=2400ppm at two superficial layers, the consumption of antiblocking agent is original 1/6, this is useful to the optical property of improving polyester film undoubtedly, has also reduced production cost simultaneously; Four, in manufacturing condition control, suitably control technological temperature, also very important to control its crystalline rate and microstructure, the present invention controls suitable technological temperature casting sheet, indulging and draw operation as far as possible, makes it non-crystallizable or few crystallization; Particularly regulate heat setting temperature in the horizontal operation of drawing, in proper range, and make it to produce microstructure with the crystallization control degree, purpose is to make it drop to minimum point to the Film Optics Effect on Performance.
The specific embodiment
Further set forth the present invention below in conjunction with specific embodiment:
Embodiment 1:
A kind of special optical level polyester film and preparation method thereof, polyester film is made through three-layer co-extruded and biaxial tension sided corona treatment, and three layers after co-extrusion stretches is two superficial layers and intermediate layer; Described intermediate layer is a polyester layer, the intermediate layer polyester is the polyester feed back of weight ratio 25% and the polyester polymers of surplus, described two superficial layers all are the silica of weight ratio 300ppm and the polyester polymers of surplus, and described polyester polymers comprises 8: 1: 5.0 phthalic acid of weight ratio, M-phthalic acid and ethylene glycol; Described silica is micron silica; Described two superficial layers respectively account for 5% of overall film thickness, and the thickness in intermediate layer accounts for 90% of total overall film thickness.
The preparation method of above-mentioned special optical level polyester film has the process of being prepared as follows:
(a) preparation process of polyester slice, phthalic acid and M-phthalic acid are made mixture by weight 8: 1 ratio, again aforesaid mixture is added in the making beating still by weight 9: 5.0 with ethylene glycol, the phosphoric acid ester stabilizing agent that adds aforesaid mixture and ethylene glycol gross weight 0.03% simultaneously, the antimony oxide catalyst of gross weight 0.03%, making beating is 30 minutes in the making beating still, import esterifying kettle then and carry out esterification, temperature control is at 220 ℃ in the esterification, 170 ℃ of fractionation column temperatures, reaction time of esterification 0.1 hour, then, carry out polycondensation reaction at 260 ℃, discharging underwater cutpellet after polycondensation reaction is finished through filtering the importing polycondensation vessel, the air-dry polyester slice of making;
(b) batch mixes, crystallizing and drying process are prepared first, second surface layer raw material and intermediate layer raw material respectively, the intermediate layer raw material be the polyester slice made in the process (a) and with the polyester feed back of polyester slice weight ratio 25%; First, second surface layer raw material is made up of polyester slice of making in the process (a) and micron silica antiblocking agent, and the weight ratio content of described silica in raw material is 300PPm; Also will give crystallization and drying to the intermediate layer raw material, giving crystallization and baking temperature is 150 ℃, and 3.5 hours time, dried intermediate layer raw material moisture content is less than 40ppm;
(c) melt extrude casting sheet process, ready raw material in the process (b) is invested extruder, extrude the continuous casting sheet with three-decker of one through the co-extrusion die head of extruder, extrusion temperature is controlled at 280 ℃, and the chilling temperature of Quench drum is controlled at below 40 ℃;
(d) longitudinal stretching process, on longitudinal stretching machine, the casting sheet is carried out twice longitudinal stretching continuously, draw ratio is 1.5: 1 for the first time, draw ratio is 2.2: 1 for the second time, and the casting sheet place of being stretched heating-up temperature is 120 ℃ during longitudinal stretching, and the casting sheet place of being stretched carries out The pre-heat treatment before the longitudinal stretching, 50 ℃ of preheat temperatures, 10 seconds preheating time, behind the longitudinal stretching film is carried out loose cooling processing, 20 ℃ of loose chilling temperatures;
(e) cross directional stretch process, on the cross directional stretch machine film after the longitudinal stretching process is being carried out cross directional stretch, cross directional stretch multiplying power 3.2: 1, the film place of being stretched temperature is 110 ℃ during cross directional stretch, the casting sheet place of being stretched carries out The pre-heat treatment before the cross directional stretch, 60 ℃ of preheat temperatures, 1 second preheating time, behind the cross directional stretch film is carried out thermal finalization and loose cooling processing, 190 ℃ of heat setting temperatures, heat-setting time 2 seconds, 80 ℃ of lax chilling temperatures;
(f) sided corona treatment process is carried out the single face sided corona treatment to film;
(g) traction wrapup procedure, film carries out rolling under the traction of carry-over pinch rolls, and the rolling mode adopts the contact rolling, and rolling pressure is 540N/M, and rolling tension force is 60N/M.
Embodiment 2:
A kind of special optical level polyester film and preparation method thereof, polyester film is made through three-layer co-extruded and biaxial tension sided corona treatment, and three layers after co-extrusion stretches is two superficial layers and intermediate layer; Described intermediate layer is a polyester layer, the intermediate layer polyester is a polyester polymers, described two superficial layers all are the silica of weight ratio 1500ppm and the polyester polymers of surplus, and described polyester polymers comprises 9: 1: 5.5 phthalic acid of weight ratio, M-phthalic acid and ethylene glycol; Described silica is micron silica; Described two superficial layers respectively account for 15% of overall film thickness, and the thickness in intermediate layer accounts for 70% of total overall film thickness.
A kind of preparation method of special optical level polyester film has the process of being prepared as follows:
(a) preparation process of polyester slice, phthalic acid and M-phthalic acid are made mixture by weight 9: 1 ratio, again aforesaid mixture is added in the making beating still by weight 10: 5.5 with ethylene glycol, the phosphoric acid ester stabilizing agent that adds aforesaid mixture and ethylene glycol gross weight 0.04% simultaneously, the antimony oxide catalyst of gross weight 0.04%, making beating is 40 minutes in the making beating still, import esterifying kettle then and carry out esterification, temperature control is at 250 ℃ in the esterification, 180 ℃ of fractionation column temperatures, reaction time of esterification 5 hours, then, carry out polycondensation reaction at 290 ℃, discharging underwater cutpellet after polycondensation reaction is finished through filtering the importing polycondensation vessel, the air-dry polyester slice of making;
(b) batch mixes, crystallizing and drying process are prepared first, second surface layer raw material and intermediate layer raw material respectively, and the intermediate layer raw material is the polyester slice of making in the process (a); First, second surface layer raw material is made up of polyester slice of making in the process (a) and micron silica antiblocking agent, and the weight ratio content of described silica in raw material is 1500PPm; Also will give crystallization and drying to the intermediate layer raw material, giving crystallization and baking temperature is 170 ℃, and 4.0 hours time, dried intermediate layer raw material moisture content is less than 40ppm;
(c) melt extrude casting sheet process, ready raw material in the process (b) is invested extruder, extrude the continuous casting sheet with three-decker of one through the co-extrusion die head of extruder, extrusion temperature is controlled at 285 ℃, and the chilling temperature of extruder chill roll is controlled at below 40 ℃;
(d) longitudinal stretching process, on longitudinal stretching machine, the casting sheet is carried out twice longitudinal stretching continuously, draw ratio is 2.0: 1 for the first time, draw ratio is 3.0: 1 for the second time, and the casting sheet place of being stretched heating-up temperature is 130 ℃ during longitudinal stretching, and the casting sheet place of being stretched carries out The pre-heat treatment before the longitudinal stretching, 120 ℃ of preheat temperatures, 5 seconds preheating time, behind the longitudinal stretching film is carried out loose cooling processing, 30 ℃ of loose chilling temperatures;
(e) cross directional stretch process, on the cross directional stretch machine film after the longitudinal stretching process is being carried out cross directional stretch, cross directional stretch multiplying power 4.2: 1, the film place of being stretched temperature is 130 ℃ during cross directional stretch, the casting sheet place of being stretched carries out The pre-heat treatment before the cross directional stretch, 105 ℃ of preheat temperatures, 3 seconds preheating time, behind the cross directional stretch film is carried out thermal finalization and loose cooling processing, 230 ℃ of heat setting temperatures, heat-setting time 5 seconds, 120 ℃ of lax chilling temperatures;
(f) sided corona treatment process is carried out two-sided sided corona treatment to film;
(g) traction wrapup procedure, film carries out rolling under the traction of carry-over pinch rolls, and the rolling mode adopts the contact rolling, and rolling pressure is 670N/M, and rolling tension force is 110N/M.
The present invention tests the performance of the special optical level polyester film of above-mentioned three embodiment, result such as following table: (film thickness is 12 microns)
Claims (2)
1. special optical level polyester film, it is characterized in that: described polyester film is made through three-layer co-extruded and biaxial tension, sided corona treatment, and three layers after co-extrusion stretches is two superficial layers and intermediate layer; Described intermediate layer is the polyester layer that contains the polyester polymers of the polyester feed back of weight ratio 0～25% and surplus, and described two superficial layers all are the polyester layer that contains the polyester polymers of the antiblocking agent silica of weight ratio 300～1500ppm and surplus; Described polyester polymers comprises weight ratio 8.0～9.0: 1: 5.0～5.5 phthalic acid, M-phthalic acid and ethylene glycol; Described antiblocking agent silica is micron order antiblocking agent silica; Described two superficial layers respectively account for 5～15% of overall film thickness, and the thickness in intermediate layer accounts for 70～90% of total overall film thickness.
2. the preparation method of special optical level polyester film as claimed in claim 1 is characterized in that having the process of being prepared as follows:
(a) preparation process of polyester slice, phthalic acid and M-phthalic acid are made mixture by weight 8.0～9.0: 1 ratio, again aforesaid mixture is added in the making beating still by weight 1: 0.50～0.55 with ethylene glycol, the phosphoric acid ester stabilizing agent that adds aforesaid mixture and ethylene glycol gross weight 0.03～0.04% simultaneously, the antimony oxide catalyst of aforesaid mixture and ethylene glycol gross weight 0.03～0.04%, in the making beating still, pulled an oar 30～40 minutes, import esterifying kettle then and carry out esterification, temperature control is at 220～250 ℃ in the esterification, 170～180 ℃ of fractionation column temperatures, reaction time of esterification 0.1～5 hour, then, carry out polycondensation reaction at 260～290 ℃, discharging underwater cutpellet after polycondensation reaction is finished through filtering the importing polycondensation vessel, the air-dry polyester slice of making;
(b) batch mixes, crystallizing and drying process are prepared first, second surface layer raw material and intermediate layer raw material respectively, the intermediate layer raw material be the polyester slice made in the process (a) and with the polyester feed back of polyester slice weight ratio 0～25%; First, second surface layer raw material is made up of polyester slice of making in the process (a) and micron order antiblocking agent silica, and the weight ratio content of described silica in raw material is 300～1500PPm; Also will give crystallization and drying to the intermediate layer raw material, giving crystallization and baking temperature is 150～170 ℃, and 3.5～4 hours time, dried intermediate layer raw material moisture content is less than 40ppm;
(c) melt extrude casting sheet process, ready raw material in the process (b) is invested extruder, extrude the continuous casting sheet with three-decker of one through the co-extrusion die head of extruder, extrusion temperature is controlled at 280～285 ℃, and the chilling temperature of Quench drum is controlled at below 40 ℃;
(d) longitudinal stretching process, on longitudinal stretching machine, the casting sheet is carried out twice longitudinal stretching continuously, draw ratio is 1.5～2.0: 1 for the first time, draw ratio is 2.2～3.0: 1 for the second time, the casting sheet place of being stretched heating-up temperature is 120～130 ℃ during longitudinal stretching, behind the longitudinal stretching film is carried out cooling and shaping and handle 20～30 ℃ of chilling temperatures;
(e) cross directional stretch process, on the cross directional stretch machine film after the longitudinal stretching process is being carried out cross directional stretch, cross directional stretch multiplying power 3.2～4.2: 1, the film place of being stretched temperature is 110～130 ℃ during cross directional stretch, the casting sheet place of being stretched carries out The pre-heat treatment before the cross directional stretch, 60～105 ℃ of preheat temperatures, 1～3 second preheating time, behind the cross directional stretch film is carried out thermal finalization and loose cooling processing, 190～230 ℃ of heat setting temperatures, heat-setting time 2～5 seconds, 80～120 ℃ of lax chilling temperatures;
(f) sided corona treatment process is carried out the single or double sided corona treatment to film, to increase surface tension;
(g) traction wrapup procedure, film carries out rolling under the traction of carry-over pinch rolls.
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| CNA2008101240492A CN101293412A (en) | 2008-05-29 | 2008-05-29 | Special optical level polyester film and production method thereof |
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