WO2007137889A2 - Procédé de production d'un film coloré en matière plastique thermoplastique, film correspondant et son utilisation - Google Patents

Procédé de production d'un film coloré en matière plastique thermoplastique, film correspondant et son utilisation Download PDF

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Publication number
WO2007137889A2
WO2007137889A2 PCT/EP2007/052406 EP2007052406W WO2007137889A2 WO 2007137889 A2 WO2007137889 A2 WO 2007137889A2 EP 2007052406 W EP2007052406 W EP 2007052406W WO 2007137889 A2 WO2007137889 A2 WO 2007137889A2
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WO
WIPO (PCT)
Prior art keywords
film
roll
colored
plastic
extrusion die
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PCT/EP2007/052406
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German (de)
English (en)
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WO2007137889A3 (fr
Inventor
Herbert Groothues
Claude Guenanten
Günther DICKHAUT-BAYER
Christoph Steinfels
Berthold SCHÖNIG
Christoph Krohmer
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Evonik Röhm Gmbh
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Publication of WO2007137889A2 publication Critical patent/WO2007137889A2/fr
Publication of WO2007137889A3 publication Critical patent/WO2007137889A3/fr

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Classifications

    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
    • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
    • G11B7/2403—Layers; Shape, structure or physical properties thereof
    • G11B7/24056—Light transmission layers lying on the light entrance side and being thinner than the substrate, e.g. specially adapted for Blu-ray® discs
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B29C48/08—Flat, e.g. panels flexible, e.g. films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/30—Extrusion nozzles or dies
    • B29C48/3001—Extrusion nozzles or dies characterised by the material or their manufacturing process
    • B29C48/3003—Materials, coating or lining therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/30—Extrusion nozzles or dies
    • B29C48/305—Extrusion nozzles or dies having a wide opening, e.g. for forming sheets
    • G—PHYSICS
    • G11—INFORMATION STORAGE
    • G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
    • G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
    • G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
    • G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
    • G11B7/252—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers
    • G11B7/254—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers of protective topcoat layers
    • G11B7/2542—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of layers other than recording layers of protective topcoat layers consisting essentially of organic resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/911—Cooling
    • B29C48/9135—Cooling of flat articles, e.g. using specially adapted supporting means
    • B29C48/914—Cooling of flat articles, e.g. using specially adapted supporting means cooling drums
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2025/00—Use of polymers of vinyl-aromatic compounds or derivatives thereof as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
    • B29K2027/06—PVC, i.e. polyvinylchloride
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2033/00—Use of polymers of unsaturated acids or derivatives thereof as moulding material
    • B29K2033/04—Polymers of esters
    • B29K2033/12—Polymers of methacrylic acid esters, e.g. PMMA, i.e. polymethylmethacrylate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2055/00—Use of specific polymers obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in a single one of main groups B29K2023/00 - B29K2049/00, e.g. having a vinyl group, as moulding material
    • B29K2055/02—ABS polymers, i.e. acrylonitrile-butadiene-styrene polymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2067/00—Use of polyesters or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2069/00—Use of PC, i.e. polycarbonates or derivatives thereof, as moulding material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2081/00—Use of polymers having sulfur, with or without nitrogen, oxygen or carbon only, in the main chain, as moulding material
    • B29K2081/04—Polysulfides, e.g. PPS, i.e. polyphenylene sulfide or derivatives thereof

Definitions

  • the invention relates to a process for the preparation of a colored, optically isotropic film made of thermoplastic materials, the film itself and the use of the film as a cover film in optical data carriers, such as the Blu-ray Disc ® and the data carrier equipped therewith.
  • EP 1 117 731 B1 describes optically virtually isotropic polycarbonate films and a chill-roll process for their preparation.
  • the films consist of linear or branched polycarbonate having an average molecular weight M w of 10,000 to 40,000.
  • Inventive films can, for. B. have a shrinkage of ⁇ 1% / ⁇ 1% (190 0 C / 30 min machine-direction (MD) / Traverse-direction (TD)).
  • MD machine-direction
  • TD Traverse-direction
  • the film according to the invention preferably does not have a deflection of linearly polarized light of greater than 2 angular minutes in any area of the surface.
  • the path difference can z. B. 31 nm, the birefringence delta n 4 x 10 -4 . In the tensile test z. B.
  • EP 1 285 742 A2 describes films for optical applications in the thickness range below 100 ⁇ m with a low phase difference of not more than 10 nm, an "optical axis deviation" of +/- 10 angular minutes and small thickness fluctuations in the range of maximum 2.4 ⁇ m per 2 cm in width
  • the films are produced by means of a chill-roll process
  • the favorable material properties are to be achieved in particular by the temperature of the polymer melt after exiting the extrusion die to the contact with the chill-roll roll at at least 30 ° C.
  • the path from the exit from the extrusion nozzle and the contact point on the chill roll can be relatively short, for example in the range of, for example, 30 to 150
  • the exiting melt film can also be thermally shielded or additionally heated by means of an enclosure Variety of plastics, especially for norbornene plastics.
  • US Pat. No. 5,476,134 describes chromium nitride-coated extruders for the production of parts from aluminum-iron alloys. These are particularly suitable for reducing the erosion of the extruded parts in the production of aluminum alloys with low iron content below 0.3
  • EP 351 886 (Bayer AG) describes a casting or extrusion process for producing optically uniaxial, birefringent polycarbonate films, which are heated by means of a quartz heater. This achieves a reduction of the unwanted birefringence to no longer disturbing values.
  • JP 8336883 describes a process for the extrusion of films of thermoplastic material, wherein an extrusion die is used, at the edges of the exit opening have a radius of 30 ⁇ m or less with an unevenness of not more than +/- 20%.
  • the nozzle geometry described counteracts in particular the formation of undesirable deposits.
  • JP 6335949 describes a process for the extrusion of films of thermoplastic material, preferably z.
  • polyethersulfones polyphenylene oxides or polyether ketones
  • an extrusion die is used, wherein the edges of the outlet opening have a radius of 30 microns or less at a non-uniformity of not more than +/- 20%.
  • the extrusion die can be made of steel or ceramic. Coatings with chromium, nickel, titanium, copper, zinc, etc. can counteract possible interactions of the nozzle material with the extruded plastic materials.
  • the nozzle geometry described counteracts in particular the formation of nozzle lines.
  • JP 2002-028941 describes a process for producing films of polyvinyl alcohol which can be used as polarizing films. Films with reduced thickness variations can be obtained by using an extrusion die in which the edges of the exit orifice have a radius of 200 ⁇ m or less.
  • JP 2003-267758 describes a process for coating optical fibers with a plastic coating.
  • an extrusion die is used, in which the edges of the outlet opening have a radius of 10 to 30 microns.
  • the nozzle geometry described counteracts in particular the formation of plastic deposit in the region of the nozzle edge, so that the method now over a longer production period can be operated trouble-free.
  • Another advantage is that the plastic coating has lower thickness variations.
  • EP 0 547 562 A1 describes a method for coating a non-descript planar web, which is transported deflected via a roller, wherein in the deflection region an extrudate is applied from a slot extrusion nozzle.
  • a distance measurement is installed to the right and left of the extrusion nozzle with a control loop. If the distance between the outlet opening of the extrusion nozzle and the roller deviates from a desired value, the position of the extrusion nozzle is correspondingly corrected by means of a servomotor.
  • the vertical birefringence of commercially available, extruded, chill-rolled polycarbonate films and commercial cast polycarbonate films is compared.
  • the extruded films have vertical birefringence values of 0.00029, the cast films values of 0.00066.
  • EP 1 327 978 (Lintec, Sony) describes a transparent cover film for optical data carriers, which is weather-resistant.
  • the cover film consists of a binder layer of acrylic polymers and the actual protective layer of polyolefins or polycarbonates.
  • the film consists of transparent polycarbonates with a thickness of 10 .mu.m to 150 .mu.m and an in-plane birefringence, which causes an optical retardation of at most 25 nm when irradiated vertically, thereby characterized in that the film in any area of the surface, based on a circular area with a diameter of 12 cm, a deflection of a perpendicularly incident light beam of greater than 0.8 angular minutes and a vertical birefringence of at most 0.0004.
  • the film has a thickness tolerance, based on a circular area with a diameter of 12 cm, of not more than +/- 1%.
  • the reflectance of the BD-ROM is set to 35% to 70% for the recording layer of a single layer BD.
  • a number of application fields for plastic films, in particular in the field of films for use as cover sheets for optical data carriers, in addition to low optical birefringence and in addition to improved surface quality of the films and lower thickness tolerances also increasingly attractive features (optical eye-catcher effects) for Markets such as film industry and video game industry.
  • EP 1 117 731 B1 and EP 1 285 742 A2 disclose remarkable solutions for the production of films with extremely low birefringence properties in the range of a few nanometers, which meet high requirements in the optical field. According to the teaching of EP 1 117 731 B1, it is possible with the surface properties to produce films which have no deflection of linearly polarized light of greater than 2 angular minutes in any area of the surface. According to EP 1 285 742 A2, thickness tolerances in the range be implemented by about 2.4 microns per 2 cm in width. The European patent applications describe transparent, undyed films, colorations are not described.
  • thermoplastic material is melted and conveyed on an extrusion line comprising an extruder, an extrusion die with an outlet opening in slot shape and a tempered roll (chill roll roll) and in the form of a flat Melt web emerges from the outlet opening of the extrusion die, the melt web is applied to the tempered roll (chill-roll roll) and cooled,
  • the tempered roller (chill-roll roller) has a concentricity of +/- 10 microns or less and the mean distance between the outlet opening extrusion die and the tempered roller (chill-roll roller) in the operating state by no more than +/- 25 ⁇ m varies over time.
  • the process of the invention is a colored film of a thermoplastic material having a thickness of 10 .mu.m to 150 .mu.m and an in-plane birefringence, which causes a vertical optical path difference of at most 15 nm when viewed vertically, and a vertical birefringence of at most 0, 0004, manufacturable or obtainable, characterized in that the film in no area of the surface, a deflection of a vertically incident light greater than an angular minute and a thickness tolerance based on a circular area with a diameter of 12 cm of not more than +/- 1%.
  • An advantage of the film according to the invention is that with it small lot sizes compared to the spin coating process when applying thin, transparent layers are easier to realize on disk.
  • a further advantage of the film according to the invention is that it is possible to provide a certificate of authenticity and origin for an exclusive coloration with a specific color mixture of the film according to the invention for certain customers.
  • This proof of authenticity can be easily seen by anyone without additional aids for everyone, by measuring the spectrum you can analyze the film at any time more precisely, if circumstances require it.
  • the function of exclusive coloring is comparable to that of a hologram.
  • the advantage of this proof of authenticity is that the colored film extends over the entire data carrier and not like a sticker that the Hologram bears, must be applied in a separate operation. The foil can not be detached from the data carrier without destruction.
  • the chill-roll melt casting process is the use of the chill-roll melt casting process, as has long been known (see, for example, EP 1 117 731 B1 or EP 1 285 742 A2).
  • a melt film emerging from an extrusion die is applied to a single cooling roll, the chill-roll roll, and cooled.
  • the melt film should not or only slightly, not more than a factor of 5 be stretched in the extrusion direction and be exposed to any active cooling before it impinges on the chill-roll roll. This has the advantage that hardly any molecular orientations occur and the resulting film has a high degree of optical isotropy.
  • the chill-roll process differs in particular from the so-called calendering processes, in which the melt film passes through a nip formed by two opposing rolls.
  • the invention relates to a process for the preparation of the colored film of the invention.
  • thermoplastic dyed plastic is melted on an extrusion line with an extruder, a melt pump and an extrusion die with an outlet opening in a slot shape, conveyed and in the form of a flat melt web ejected from the outlet opening of the extrusion die.
  • thermoplastic material can be done by any conventional method. Preferred is the use of a masterbatch, i. a premix of the plastic to be extruded with the dye to be used, wherein the dye concentration in the master batch is higher than in the finally colored plastic film.
  • a melt filter is provided between the melt pump and the extrusion die, which retains impurities.
  • the mesh size of the filter insert can, for. B. 5 microns to 50 microns, preferably z. B. 10 microns to 30 microns.
  • the extrusion die can furthermore be provided in the nozzle exit region in a manner known per se with a profile tool.
  • the profile tool is used for fine adjustment of the exiting colored melt profile by a thin-walled designed exit area under pressure of actuators, eg. As bolts, expansion bolts or piezotranslators, is deformed accordingly. Suitable is z.
  • actuators eg. As bolts, expansion bolts or piezotranslators
  • Suitable is z.
  • the execution of the nozzle exit area as a flexible lip or as a so-called “superflex lip” (see, for example, EP-A 367 022) or as a membrane (see, Gross et al., Plastics 84 (1994) 10, pp 1352-1358).
  • the dyed melt web is applied to a single cooled roll, called a chill roll roll, and cooled.
  • the chill roll can be z. B. have a temperature of 100 0 C to 200 0 C, preferably from 100 ° C to 130 0 C. Avoidance of vibration transmission
  • the invention is based on the finding that vibrations can be transmitted to the extrusion nozzle from the area of the extruder and in particular the melt pump. These vibrations result in varying operating distances between the outlet opening of the extrusion die and the chill-roll roll. The varying distances in turn lead to compressions or elongations of the colored melt web, which in turn leads to an increase in thickness tolerances.
  • the invention is further based on the finding that the chill-roll roll contributes to its own imbalance at varying distances between the outlet opening of the extrusion die and the chill-roll roll.
  • the varying distances in turn lead to compressions or elongations of the colored melt web, which in turn leads to an increase in thickness tolerances.
  • an extrusion plant in which the cooled roll (chill-roll roll) a Concentricity of +/- 10 microns or less, preferably of +/- 5 microns or less, and the mean distance between the outlet opening of the extrusion die and the cooled roll (chill-roll roll) in the operating state by not more than + / - 25 microns, preferably by not more than +/- 15 microns, more preferably not changed by more than +/- 10 microns.
  • suitable temperature-controllable rollers (chill roll) with a concentricity of +/- 10 microns or less, preferably from +/- 5 microns can be manufactured in this accuracy and are available from manufacturers of parts for extrusion equipment.
  • the specified runout accuracy refers to the installed state or to the operating state. The roller must therefore be both accurately manufactured and positioned and centered with high accuracy in the extrusion line.
  • the average distance or the respective minimum distance between the outlet opening of the extrusion die and the cooled roll can, for. B. be determined by means of optical measuring sensors or by Laserwegeflop practically between any selected measuring points. It does not depend on the distance itself, but on the temporal variation of the distance.
  • the average distance is measured by two temperature-independent distance sensors, which are respectively positioned to the right and left of the outlet opening of the extrusion die, so that they can capture from there, preferably the shortest distance or the shortest distances to tempered roller.
  • a technical measure may be, the roll mill holding the tempered roll (chill-roll roll), at one or more points z. B. via braces, z. As steel, fixed to the extrusion die, z. B. by screwing or riveting to connect.
  • a further technical measure may be to connect the roll mill holding the cooled roll (chill-roll roll) to the extrusion die via at least two actuators, the actuators being controlled via a control loop so as to actively change the distance between the exit orifice Counteract the extrusion die and the tempered roll.
  • the actuators, z. B. piezo actuators, z. B. be installed right and left of the tempered roller and connected at points right and left of the outlet opening of the extrusion die with this. If necessary, additional fixed braces can also be attached between the roll mill and the extrusion die.
  • the extrusion line has a melt pump between the extruder and the extrusion die.
  • the melt pump brings about a leveling of the otherwise fluctuating melt pressure from the extruder into the extrusion nozzle and thus likewise contributes to the reduction of vibration transmissions.
  • an extrusion plant is used in which the melt pump is decoupled from the extrusion die to avoid vibration transmission.
  • the decoupling can be accomplished mechanically, z. B. over flexible, high temperature resistant lines for the colored melt.
  • a reduction or avoidance of the vibration transmission from the melt pump to the extrusion die has the advantage that dyed films can be obtained with further reduced thickness tolerances and improved surface quality.
  • the radius of the edges of the outlet opening of the extrusion die of at most 50 .mu.m, preferably of at most or less than 30 .mu.m, in particular of at most or less than 25 microns.
  • the radii of the edges of the outlet opening of the extrusion nozzle preferably have an unevenness of at most or less +/- 5% over the width of the outlet opening.
  • the comparatively sharp and very uniform edges probably lead to a particularly good detachment of the melt web, which can contribute to the preservation of films with low thickness tolerances.
  • the edge or both edges of the outlet opening at an angle of 45 to 100 °, usually of 90 °.
  • the roughness of the inner surface of the die lip area can affect the surface quality of the films produced.
  • the inner surface of the die lip area is the area behind the distribution channel and an optional jam island.
  • the inner surface of the die lip region extends approximately 0.5 cm to 5 cm from the outlet opening into the interior of the extrusion die.
  • the inner surface of the die lip region should preferably have roughness R 3 to DIN 4768 of 0.01 .mu.m to 0.002 .mu.m or less, R z of 0.08 .mu.m to 0.015 .mu.m and R max 0.10 .mu.m to 0.025 .mu.m.
  • the inner surface of the die lip portion of the extrusion die is provided with a friction reducing coating.
  • a friction reducing coating is provided.
  • Favorable coatings are having a total thickness in the range of 10 .mu.m to 30 .mu.m, preferably from 15 .mu.m to 25 .mu.m.
  • the lip region of the nozzle is preferably subdivided into separable elements, thus allowing better accessibility in the processing of the inner surface.
  • the preferred roughness depth range can be achieved by polishing or by coating the inner surface of the die lip area.
  • the inner surface of the nozzle lip region z. B. be equipped with a chrome plating, which can be additionally polished.
  • the coating may preferably consist of Ni, CrN, TiCN, TiC, TiAIN, DLC (diamond-like carbon) or another diamond-like carbon coating. These coatings have the advantage of higher, up to ten times longer service life compared to a chromium coating as described in EP 1 117 731 B1. Corresponding coatings and their application to steel surfaces are known in the art in principle, for. From US 5,476,134 or US 4,637,477.
  • a suitable method for applying a corresponding coating to the inner surface of the die lip area is z.
  • the "physical vapor deposition" method PVD method, see, for example, US Pat. No. 5,476,134 or US Pat. No. 4,637,477)
  • the coating can be single-layer or preferably multi-layered In the multilayer coating, the comparatively soft steel or steel alloy
  • a hard layer eg a 10 ⁇ m to 20 ⁇ m thick layer of nickel, which is then coated with an even harder layer, eg a 2 ⁇ m to 5 ⁇ m thick layer of TiN, CrN or DLC, is preferably applied to the extrusion die
  • a multilayer coating of the inner surface of the inner nickel layer and a layer of TiN, CrN or DLC coated thereon is particularly advantageous for the extrusion of polycarbonate films, and the inner surface of the extrusion die in the extrusion die lip region can be metallurgically or chemically altered or be doped.
  • the inked melt web is heated on the way between the exit from the extrusion die and the touchdown point on the chill-roll roll.
  • This has the advantage that internal molecular stresses occur only reduced. It is advantageous to heat the dyed melt web so that it at or shortly before the touchdown on the chill roll a temperature of at least 30 0 C, at least 40 0 C, at least 50 0 C, at least 60 ° C or at least Having 80 ° C above the glass transition temperature of the extruded plastic.
  • glass temperature is meant in particular the midpoint temperature T mg according to ISO 11357-2, point 3.3.3.
  • the measurement is carried out without addition of plasticizer, with residual monomer contents (REMO) of less than 100 ppm, at a heating rate of 10 ° C / min and under a nitrogen atmosphere.
  • REMO residual monomer contents
  • An extrusion line is preferably used or used in which the colored melt web is surrounded by an enclosure between the exit from the extrusion die and the touchdown point on the chill roll roll.
  • this enables effective heating of the colored melt web and at the same time opens up the possibility of the inked melt web on the way between the exit from the extrusion die and the landing point on the chill-roll roll with an inert gas, e.g. As nitrogen, to surround.
  • an inert gas e.g. As nitrogen
  • the invention relates to a colored film of a thermoplastic material having a thickness of 10 .mu.m to 150 .mu.m, preferably 20 .mu.m to 120 .mu.m, in particular 30 .mu.m to 100 .mu.m.
  • the in-plane birefringence of the inked film is calculated from the optical retardation.
  • the optical path difference due to the birefringence of a, with respect to the film surface perpendicular incident light beam z. B. according to the principle of polarization microscopy (polarimeter) can be determined.
  • the methodology is familiar to the person skilled in the art (see, for example, ISO 11455).
  • the colored film has a birefringence (in-plane birefringence), the vertical transmission a optical retardation of at most 15 nm, preferably at most 5 nm, it can, for. B. 2 nm to 10 nm or 2 nm to 5 nm. Colored films with these values are called optically and mechanically isotropic or nearly isotropic and are suitable for optical applications with high requirements.
  • Vertical birefringence in-plane birefringence
  • the colored extruded film according to the invention differs, among other things, from cast films (see, for example, EP 351 886), by a significantly lower vertical birefringence (see, for example, EP 1 202 261 A1).
  • the vertical birefringence of the colored film according to the invention is at most 0.0004, preferably at most 0.0003.
  • a suitable measurement method for determining the vertical birefringence is z. In detail in EP 1 202 261 A1, p. 11, line 44 - p. 12, line 24. In contrast to the in-plane birefringence measurement, the principle is based on a light incidence angle of 45 °.
  • a low value in the vertical birefringence is particularly advantageous when the colored film according to the invention is used in optical data carriers.
  • the signal-to-noise ratio degrades with increasing vertical birefringence.
  • the colored film does not have a deflection of a vertically incident light beam of greater than in any area of the surface, based on a circular area with a diameter of 12 cm, preferably based on an area of 1 m 2 , more preferably based on an area of 10 m 2 as an angular minute, preferably not more than 0.5 angular minutes.
  • the measurement is carried out by means of the registration of the deflection angle, which is experienced by a laser beam of about 200 ⁇ m diameter, which penetrates the colored foil. For this purpose, the so-called laser deflection method is used.
  • the angular deviation is measured by means of a displacement table operated with a stepper motor, which is experienced by a laser beam of about 100 ⁇ m in diameter when the colored foil is irradiated vertically.
  • punched pieces with a circular area with a diameter of 12 cm or sections or sections of the film web of 1 or 10 m 2 can be measured.
  • the inked film has a thickness tolerance or difference in the thickness of the film, based on a circular area with a diameter of 12 cm, of not more than +/- 1%, preferably not more than +/- 0.5% ,
  • the percentage deviation refers to the mean of the maximum and the minimum thickness value within the circular area with a diameter of 12 cm.
  • This specification ensures that the film z. B. for the production of optical data storage with high storage density of z. B. 25 gigabytes (GB) or more is suitable.
  • the thickness deviation from the mean value is accordingly no more than +/- 1 ⁇ m within a circular area with a diameter of 12 cm.
  • the determination of the thickness tolerance can be determined by interferometric layer thickness measurement, which is known to the person skilled in the art.
  • interferometric layer thickness measurement z.
  • an achromatic measuring head can be used.
  • the layer thickness measurement is based on the superimposition of the light reflected at both boundary surfaces of the colored film. With a known refractive index of the material, the layer thickness can be determined from the spectrum of the reflected light.
  • the colored film consists of a thermoplastic, preferably of transparent thermoplastic material.
  • the non-colored film has a light transmittance for daylight (standard illuminant D65) T D65 SZB DIN 5033/5036 in the range of at least 60%, preferably from 65 to 92%.
  • the colored film can, for. B. from polymethyl methacrylate plastic, impact modified polymethylmethacrylate, polycarbonate plastic, polystyrene plastic, styrene-acrylonitrile plastic, polyethylene terephthalate plastic, glycol-modified polyethylene terephthalate plastic, polyvinyl chloride plastic, polyolefin plastic, cycloolefinic copolymers (COC), P PS plastic or PPSU plastic, acrylonitrile-butadiene-styrene (ABS) plastic or mixtures (blends) of various thermoplastic materials.
  • polymethyl methacrylate plastic impact modified polymethylmethacrylate
  • polycarbonate plastic polystyrene plastic
  • styrene-acrylonitrile plastic polyethylene terephthalate plastic
  • glycol-modified polyethylene terephthalate plastic glycol-modified polyethylene terephthalate plastic
  • polyvinyl chloride plastic polyolefin plastic
  • the inked film preferably consists of a linear or branched polycarbonate having an average molecular weight Mw (weight average) of from 10,000 to 45,000, preferably from 12,000 to 25,000, particularly preferably from 15,000 to 20,000.
  • Mw average molecular weight
  • the molecular weight M w (weight average) can be determined, for example, by gel permeation chromatography or by scattered light method (see, for example, BHF Mark et al., Encyclopaedia of Polymer Science and Engineering, 2nd Edition, Vol , 1989).
  • Dyes which can be used are all dyes which are compatible with polycarbonates and can be dispersed very well.
  • dyes from Clariant Sandoplast dyes such as Orange 3G, Red PFS, Red Violet R, Blue 2B, Green G
  • dyes from Ciba Sandoplast dyes such as Orange 3G, Red PFS, Red Violet R, Blue 2B, Green G
  • equivalent dyes from Ciba for example, to dyes from Clariant (Sandoplast dyes such as Orange 3G, Red PFS, Red Violet R, Blue 2B, Green G) or, for example, equivalent dyes from Ciba.
  • the colored film of the invention may, for. B. for the construction of transparent, colored layers in optical media, as a colored cover of optical media, as a colored cover for scratch protection of optical media, as a colored carrier material for the information layer of optical media or as a colored functional film in liquid crystal displays. Furthermore, the film can be used as proof of authenticity or origin. For this purpose, it is colored individually.
  • the extrusion plant consists of a single-screw extruder, a melt pump and a slot-type extrusion die with an outlet opening of 680 mm x 0.4 mm.
  • the slot-type extrusion die is designed as a superflex lip (see EP-A 367 022).
  • the inner surface of the extrusion nozzle in the lip area is polished, so that a roughness Ra of 0.002 ⁇ m, Rz of 0.015 ⁇ m and Rmax of 0.025 ⁇ m is achieved.
  • the inner surface of the extrusion die is provided with a duplex coating of 15 ⁇ m nickel and 5 ⁇ m CrN.
  • the radius of the die lip in the exit region is between approximately 100 and 200 ⁇ m and has a radius uniformity of +/- 50 ⁇ m across the width.
  • a chill-roll roll is positioned in the center.
  • the roller has a diameter of 400 mm and a width of 700 mm.
  • the extrusion die is firmly connected to the roll mill at two points on the right and left of the outlet opening of the extrusion die via steel profile beams with a cross section of 5 cm ⁇ 1 cm.
  • the temperature of the chill-roll roller is set between 100 0 C and 130 0 C, preferably 110 ° C to 120 0 C.
  • the temperature of the colored melt stream is about 240 0 C.
  • the colored melt film places approximately tangentially to the roll surface and wraps around the roller at approximately 180 ° C.
  • the distance between the outlet of the colored melt from the nozzle and the contact point to the chill-roll roll is housed, the internal temperature is about 120 0 C.
  • This enclosure can be heated or under a protective gas atmosphere, eg heated and filtered (clean room class 100 ) Nitrogen, be filled.
  • the thickness of the inked film web is determined by a traversierend arranged, non-contact measuring system and regulated by means of electronically processed information, the melt distribution of the nozzle by means of a Dehnbolzensystems across the width.
  • Example 1 Reference samples of polycarbonates without coloring
  • Examples 2, 3 and 4 were made with Clariant Sandoplast Blue 2B
  • Examples 5 and 6 were made with Clariant Sandoplast Green G
  • Examples 7 and 8 were made with Clariant Sandoplast Red PFS
  • the relevant measured quantities of the dyed films obtained in Examples 1 to 8 are determined by means of punched-out circular colored surface pieces with a diameter of 12 cm and are summarized in the following table.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

L'invention concerne un procédé de production d'un film coloré en matière plastique thermoplastique, procédé dans lequel ladite matière plastique thermoplastique est fondue et transportée dans une installation d'extrusion comprenant une extrudeuse, une filière d'extrusion à ouverture de sortie se présentant sous la forme d'une filière plate, et un cylindre à température réglable (cylindre refroidisseur) fixé sur un support de cylindre, puis sort de l'ouverture de sortie de la filière d'extrusion sous la forme d'une bande fondue colorée plane, ladite bande est appliquée et refroidie sur le cylindre à température réglable (cylindre refroidisseur), caractérisé en ce que le cylindre à température réglable (cylindre refroidisseur) présente une précision de concentricité de +/- 10 μm, ou moins, et en ce que la distance moyenne entre l'ouverture de sortie de la filière d'extrusion et le cylindre à température réglable (cylindre refroidisseur) varie, dans le temps, en cours du fonctionnement, au maximum de +/- 25 μm. L'invention concerne en outre le film coloré proprement dit, ainsi que ses utilisations comme film coloré pour des supports de données.
PCT/EP2007/052406 2006-05-30 2007-03-14 Procédé de production d'un film coloré en matière plastique thermoplastique, film correspondant et son utilisation WO2007137889A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102006025481.3 2006-05-30
DE102006025481A DE102006025481A1 (de) 2006-05-30 2006-05-30 Verfahren zur Herstellung einer eingefärbten Folie aus thermoplastischem Kunststoffen, Folie und Verwendung der Folie

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WO2007137889A3 WO2007137889A3 (fr) 2008-01-24

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CN113811449A (zh) * 2020-04-07 2021-12-17 法国圣戈班玻璃厂 具有楔形截面的着色热塑性中间层

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DE102010062900A1 (de) * 2010-12-13 2012-06-14 Evonik Röhm Gmbh Verfahren zur Herstellung von Lichtleitkörpern und deren Verwendung in Beleuchtungseinheit

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WO2002029801A1 (fr) * 2000-09-29 2002-04-11 General Electric Company A Corporation Of The State Of New York Support de stockage de donnees colore
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EP1117731B1 (fr) * 1998-08-14 2003-02-26 Röhm GmbH & Co. KG Films en polycarbonate optiquement isotropes, ainsi que leur procede de fabrication
EP1454741A2 (fr) * 2003-03-07 2004-09-08 Klöckner Pentaplast B.V. Feuille en matière plastique pour meuble
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US6099930A (en) * 1996-12-17 2000-08-08 Isotag Technology, Inc. Methods for marking digital compact discs as a means to determine its authenticity
JP2002260282A (ja) * 2001-03-01 2002-09-13 Ricoh Co Ltd 光記録媒体
US6475589B1 (en) * 2001-12-17 2002-11-05 General Electric Company Colored optical discs and methods for making the same
DE102004022673A1 (de) * 2004-05-07 2005-11-24 Bayer Materialscience Ag Copolycarbonate mit verbesserter Fließfähigkeit

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US3422494A (en) * 1964-10-19 1969-01-21 Du Pont Apparatus for forming layers
DD152817A1 (de) * 1980-08-28 1981-12-09 Klaus Berghof Verfahren zur herstellung spinnmassegefaerbter foliefaeden
EP1117731B1 (fr) * 1998-08-14 2003-02-26 Röhm GmbH & Co. KG Films en polycarbonate optiquement isotropes, ainsi que leur procede de fabrication
WO2002029801A1 (fr) * 2000-09-29 2002-04-11 General Electric Company A Corporation Of The State Of New York Support de stockage de donnees colore
EP1202261A1 (fr) * 2000-10-24 2002-05-02 3M Innovative Properties Company Support d'enregistrement optique
US6475588B1 (en) * 2001-08-07 2002-11-05 General Electric Company Colored digital versatile disks
EP1454741A2 (fr) * 2003-03-07 2004-09-08 Klöckner Pentaplast B.V. Feuille en matière plastique pour meuble
US20050013965A1 (en) * 2003-05-09 2005-01-20 Tdk Corporation Optical recording medium
DE102005020424A1 (de) * 2005-04-29 2006-11-02 Röhm Gmbh Verfahren zur Herstellung einer Folie aus thermoplastischem Kunststoff, Folie und Verwendung der Folie

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CN113811449A (zh) * 2020-04-07 2021-12-17 法国圣戈班玻璃厂 具有楔形截面的着色热塑性中间层

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