WO2011043285A1 - 熱可塑性樹脂フィルムの製造方法及び製造装置 - Google Patents
熱可塑性樹脂フィルムの製造方法及び製造装置 Download PDFInfo
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- WO2011043285A1 WO2011043285A1 PCT/JP2010/067348 JP2010067348W WO2011043285A1 WO 2011043285 A1 WO2011043285 A1 WO 2011043285A1 JP 2010067348 W JP2010067348 W JP 2010067348W WO 2011043285 A1 WO2011043285 A1 WO 2011043285A1
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- spray nozzle
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- 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
- B29C48/915—Cooling of flat articles, e.g. using specially adapted supporting means with means for improving the adhesion to the supporting means
- B29C48/917—Cooling of flat articles, e.g. using specially adapted supporting means with means for improving the adhesion to the supporting means by applying pressurised gas to the surface of the flat article
-
- 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
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- 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
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- 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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/50—Details of extruders
- B29C48/76—Venting, drying means; Degassing means
- B29C48/768—Venting, drying means; Degassing means outside the apparatus, e.g. after the die
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- 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
- B29C2948/00—Indexing scheme relating to extrusion moulding
-
- 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
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2007/00—Flat articles, e.g. films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2011/00—Optical elements, e.g. lenses, prisms
- B29L2011/0075—Light guides, optical cables
Definitions
- the present invention relates to a manufacturing method and a manufacturing apparatus for an optical film, in particular, having few surface foreign matter defects and having excellent uniformity in optical characteristics.
- the optical film is made of various transparent films made of thermoplastic resin such as polyester such as polyethylene terephthalate (PET), acrylic polymer, polycarbonate (PC), etc., for protection, for example, to prevent damage. It is obtained by applying various surface treatments to laminate a film (hard coat layer), AR layer (antireflection layer), light collecting / light diffusing layer, polarizing plate, etc. on the substrate. There is a strong demand for transparency. On the other hand, when it is processed by being incorporated into a large display or the like, a sufficient thickness is required, so that a thick film having a thickness of 150 ⁇ m or more is preferably used.
- thermoplastic resin such as polyester such as polyethylene terephthalate (PET), acrylic polymer, polycarbonate (PC), etc.
- the manufacturing process of such a film includes a process of extruding a molten thermoplastic resin from an extrusion die and cooling it, and in order to manufacture a film having excellent transparency, the extruded thermoplastic resin is quickly desired. It is important to cool to temperature.
- a method for quickly cooling the thermoplastic resin a method of bringing the thermoplastic resin into close contact with the cooling drum is generally used.
- a film surface that is not in contact with the cooling drum (anti-cooling drum) It is also necessary to cool from the surface. This is because, in a thick film, when cooling with only a cooling drum, the film temperature on the surface of the anti-cooling drum does not easily fall to a desired temperature.
- auxiliary cooling device is installed on the surface of the anti-cooling drum and the cooling of the molten thermoplastic resin is promoted.
- This auxiliary cooling device is generally constituted by, for example, a nozzle (hereinafter referred to as a spray nozzle) that blows cool air from the surface of the anti-cooling drum toward the thermoplastic resin (for example, Patent Document 1).
- thermoplastic resin such as a resin such as polyester
- a resin such as polyester
- the oligomer volatilized around the auxiliary cooling device is deposited, for example, on the surface of the spray nozzle of the auxiliary cooling device or the exhaust surface. Oligomer deposited on the surface of the auxiliary cooling device may be guided by the blowing air of the auxiliary cooling device and fall and adhere to the film surface, resulting in a foreign matter defect.
- the cooling rate does not increase and the transparency of the film is increased. descend.
- the tip of the spray nozzle is moved as close as possible to the thermoplastic resin film, the cooling speed increases, but the oligomer is deposited on the auxiliary cooling device, and the oligomer is sprayed on the thermoplastic resin film and adheres to the surface of the thermoplastic resin film. As a result, foreign matter defects and troubles in the subsequent process are caused.
- thermoplastic resin film when the molten thermoplastic resin is cast on a cooling drum and cooled and solidified on the cooling drum to form a thermoplastic resin film, the film is transferred from the anti-cooling drum surface to the film.
- an inter-nozzle exhaust mechanism including a shut-off plate having a plurality of exhaust holes while blowing cooling air by an air supply means including a spray nozzle extending in the width direction of the cooling drum in the previous period Is known, and a method for producing a thermoplastic resin film is known in which the air supply and exhaust means are alternately performed in the film flow direction (for example, Patent Document 2).
- the cooling air blowing nozzle and the suction surface of the exhaust mechanism are connected to the cooling drum. It is installed alternately along the rotation direction. At that time, the ratio of the total suction air volume of all suction surfaces to the total air volume of all spray nozzles is set to 3.4 to 4.5, and the air in the oligomer atmosphere is actively removed. Cooling methods are known. Also, a technique is known in which a heater for preventing oligomer precipitation is provided at least on the wall surface inside the first suction surface of the exhaust mechanism with respect to the oligomer around the auxiliary cooling device (for example, Patent Document 3).
- the cooling device Accordingly, as the usage time of the cooling device elapses, the amount of oligomers deposited on the suction surface of the exhaust mechanism increases, and the deposited oligomers fall on the surface of the thermoplastic resin film, causing foreign matter defects. As a result, due to the increase in the defect of such foreign matter over time, a defect loss in use of the auxiliary cooling device occurs, and the production rate is lowered.
- JP-A-3-239525 Japanese Patent No. 3334451 JP 2006-281531 A JP-A-7-329153
- An object of this invention is to provide the manufacturing method and manufacturing apparatus of a thermoplastic resin film which can suppress precipitation and deposition of the oligomer to a spray nozzle, the exhaust mechanism between nozzles, etc., maintaining high cooling efficiency.
- the present inventors have completed the present invention by an advanced combination of the design of an auxiliary cooling device for cooling and solidifying a molten thermoplastic resin and the setting of process conditions including a preferable indoor environment at the time of production. . That is, in order to solve the problems of the prior art, when casting the molten thermoplastic resin from the extrusion die onto the cooling drum, a spray nozzle and a suction / discharge mechanism are provided, and the film surface (hereinafter referred to as the cooling drum) In the device configuration that sucks air in the vicinity of the film while cooling the anti-cooling drum surface), the balance between the blowing air volume and the suction / discharge amount, and the supply / exhaust of the entire chamber including the cooling drum and auxiliary cooling device Balance optimization is the means to achieve it.
- the object of the present invention can be achieved by the following means.
- a molten thermoplastic resin is cast on a cooling drum from an extrusion die, and is cooled and solidified on the cooling drum to produce a thermoplastic resin film.
- a device that sucks air near the film from the anti-cooling drum surface by the inter-nozzle exhaust mechanism while simultaneously blowing air from the cooling drum surface toward the film by the spray nozzle, and the suction surface of the inter-nozzle exhaust mechanism Is installed at a position away from the film from the front end surface of the spray nozzle, and another is an apparatus for producing a thermoplastic resin film, wherein the molten thermoplastic resin is placed on a cooling drum from an extrusion die.
- thermoplastic resin film When the film is cast and cooled and solidified on the cooling drum to produce a thermoplastic resin film, the film surface not contacting the cooling drum (hereinafter referred to as anti-cooling drum)
- a method for producing a thermoplastic resin film having a step of simultaneously sucking air in the vicinity of the film from the surface of the anti-cooling drum while blowing air toward the film from the surface).
- S is a method for producing a thermoplastic resin film, wherein S is greater than or equal to E, where E is the total amount of air to be sucked per unit time.
- the amount of air blown by the main cooling device on the surface of the anti-cooling drum is made larger than the suction amount, so that air with a high oligomer concentration around the extrusion die is not sucked into the main cooling device.
- the device of the present invention may be referred to as the present cooling device.
- the suction / discharge mechanism at a position farther from the film than the tip of the spray nozzle, even if some oligomer is deposited on the suction surface, it is difficult for the oligomer to fall and adhere to the film surface.
- the cooling efficiency of the spray nozzle can be secured, and crystallization scratches are less likely to occur.
- an exhaust mechanism is provided on the surface of the anti-cooling drum and around the extrusion die so that the supply / exhaust balance of the entire chamber is excessively exhausted.
- the air that is blown from and blown up in the direction of the extrusion die is discharged.
- the film obtained by the present invention has been solved at the same time, the problem of surface foreign matter caused by oligomers, the problem of crystallization scratches, which has been difficult to achieve with conventional techniques for manufacturing thick films having a film thickness of about 150 ⁇ m or more, It is mainly suitable for display-related applications, in particular, as a light diffusion layer for diffusion plates, a prism layer for prism sheets, an antireflection layer for antireflection films, and a substrate for optical functional films used for polarizing plate processing. .
- thermoplastic resin film in connection with this invention. It is an enlarged view of the spray nozzle of FIG. It is a schematic side view of the best inter-nozzle exhaust mechanism position according to the present invention.
- thermoplastic resin film obtained by the method for producing a thermoplastic resin film of the present invention may be a polyester such as polyethylene terephthalate (hereinafter sometimes abbreviated as PET), an acrylic polymer, or a polycarbonate (hereinafter abbreviated as PC). ).
- PET polyethylene terephthalate
- PC polycarbonate
- thermoplastic resin film of the present invention As a method for producing the thermoplastic resin film of the present invention, as shown in a schematic side view in FIG. 1 and a partially enlarged view of FIG. 1 in FIG. 2, for example, an extrusion die 1 and a cooling drum 2 just below it are provided.
- the blowing nozzle 6 As the main cooling device on the anti-cooling drum surface along the rotation direction of the cooling drum 2, the blowing nozzle 6 is arranged so as to blow air toward the center of the cooling drum 2, and the circumference of the cooling drum 2 Arranged in the direction.
- the extrusion die peripheral exhaust mechanism 5 may be installed upstream of the extrusion die (on the side where the molten thermoplastic resin is cast) and on the upper part of the inter-nozzle exhaust mechanism.
- the molten thermoplastic resin when the molten thermoplastic resin is cast from the extrusion die 1 onto the cooling drum 2 to the thermoplastic resin film 3 having a thickness of about 1 to 5 mm and cooled and solidified, the molten thermoplastic resin is directed toward the anti-cooling drum surface of the film.
- Two or more spray nozzles 6 for spraying air are provided (the total amount of air from the plurality of spray nozzles per unit time is S.
- the blowing air S is made larger than the suction air E (S> E) or equalized so that the air having a high oligomer concentration around the extrusion die is blown to the blowing nozzle and the cooling drum. Avoid as much as possible between them.
- the suction air E is preferably in the range of 25 to 150 m 3 / min, more preferably 40 to 80 m 3 / min.
- the blowing air S is preferably in the range of 50 to 150 m 3 / min, more preferably 70 to 100 m 3 / min.
- the relationship between the suction air E and the spray air S is set so that the spray air S is larger than or equal to the suction air E, but the ratio E / S is preferably 0.5 to 1.0, more preferably 0.8. It is in the range of 5 to 0.9.
- this ratio is larger than 1.0, an air flow is formed between the cooling device and the cooling drum so as to suck high concentration oligomer air around the extrusion die.
- this ratio is less than 0.5, the blow-up increases, and the thermoplastic resin may vibrate between the time it is pushed out of the extrusion die and landing on the cooling drum, which may cause uneven thickness. is there.
- the apparatus or the manufacturing method of the present invention it is desirable that high-concentration oligomer air staying around the extrusion die is sucked and discharged by another exhaust mechanism as indicated by 5 in FIG.
- the position of the extrusion die peripheral exhaust mechanism for example, it is preferable to install it on the anti-cooling drum surface of the film such as the ceiling of the casting chamber and on the upper side of the cooling drum.
- the spray nozzle and the inter-nozzle exhaust mechanism of the device of the present invention for example, the spray nozzle extending in the width direction of the cooling drum and the suction surface of the inter-nozzle exhaust mechanism are alternately arranged along the rotation direction of the cooling drum,
- the inter-nozzle exhaust mechanism exists as a blocking plate having a plurality of exhaust holes.
- the spray nozzle has nozzles with slit-shaped tip portions with a gap of 2 to 10 mm at a pitch of 100 to 150 mm and 5 to 15 in the circumferential direction.
- a configuration in which steps are installed is preferably exemplified.
- the film region having a high crystallization speed cannot be cooled, and crystallization flaws may occur.
- the width of the spray nozzle is preferably 100 to 500 mm wider than the width of the thermoplastic resin film on the cooling drum.
- the distance between the tip surface of the spray nozzle and the surface of the thermoplastic resin film is preferably 5 to 30 mm.
- the distance between the tip surface of the spray nozzle and the film is less than 5 mm, the film surface is likely to be deformed by the spray air, and oligomers are also likely to adhere to the film surface.
- this distance is more than 30 mm, the cooling efficiency of the blowing air is lowered, and there is a possibility that crystallization scratches are generated.
- the position of the first spray nozzle is preferably a position where the length 10 along the rotation direction of the cooling drum from directly above the top of the cooling drum to the landing point of the blowing air of the first spray nozzle is 500 mm or more, More preferably, it should be installed at a distance of 1000 mm or more. If the distance is closer than 500 mm, the melted thermoplastic resin flowing from the extrusion die causes film shaking, and there is a problem that surface unevenness occurs in the film.
- the holes on the suction surface of the inter-nozzle exhaust mechanism preferably have a hole diameter of 4 to 10 mm, and the number of rows is 5 to 10 with respect to one suction surface. If the hole diameter is smaller than 4 mm and there are more than 10 rows, the pressure loss around the holes during suction increases, exhaust air cannot be sucked, and oligomers tend to accumulate.
- the width should be matched to the width of the spray nozzle.
- the spray nozzle in the uppermost part.
- oligomers are deposited and deposited on the suction surface, and easily fall on the film surface, which easily causes foreign matter defects.
- a material with low surface friction such as diamond coating (DLC)
- DLC diamond coating
- oligomer precipitation preventing process on the tip surface of the spray nozzle and the suction surface of the inter-nozzle exhaust mechanism.
- DLC diamond coating
- it can be applied inexpensively and easily by attaching a fluororesin coating or a fluororesin tape to the surface.
- the tip surface of the spray nozzle is preferably exemplified by a slit type having slit-like openings with a constant gap in the width direction, a perforated plate type having a plurality of circular holes, and the like.
- the perforated plate type is generally higher than the slit type if the opening area of the tip surface of the spray nozzle and the wind speed and temperature of the spray air are the same (for example, Patent Document 4).
- Patent Document 4 Patent Document 4
- the effect of preventing crystallization scratches is great.
- the hole diameter or the hole-to-hole interval is too large, cooling unevenness may occur.
- the jets of the spray nozzles interfere with each other and the jets are likely to fluctuate, resulting in reduced cooling efficiency and uneven cooling.
- the area of the tip surface of the spray nozzle increases, and oligomers are likely to precipitate and accumulate. . Therefore, it is preferable to design the tip face of the spray nozzle so that the area of the tip face of the spray nozzle is as small as possible while considering the cooling efficiency.
- the hole diameter is preferably 2 to 10 mm
- the number of rows per spray nozzle is preferably 2 to 6 rows.
- the selection of the perforated plate type and the slit type of the spray nozzle may be determined in consideration of various conditions depending on the crystallization characteristics of the thermoplastic resin, the cooling drum specifications, the strength of the desired cooling air, and the degree of cooling.
- a slit nozzle is installed at the uppermost stage as an air curtain that suppresses the suction of air from around the extrusion die, and the perforated plate is placed in a temperature range where the crystallization speed is high. It is better to install a spray nozzle to increase cooling efficiency.
- the suction surface of the inter-nozzle exhaust mechanism uses a shielding plate with a plurality of holes so that air in the vicinity of the film is sucked from the exhaust holes without stagnation and is generated from the film and floats in the air in the vicinity of the film. Can be quickly sucked out of the exhaust hole and discharged out of the system.
- oligomers may be deposited and deposited on the suction surface, for example, the edge of the exhaust hole, and if the oligomers fall and adhere to the film surface due to the blowing air, there is a possibility that a foreign matter defect may occur. Therefore, as shown in FIG.
- the suction surface 8 of the inter-nozzle exhaust mechanism is preferably installed farther from the cooling drum than the tip surface 9 of the nozzle. Further, the distance from the suction surface of the inter-nozzle exhaust mechanism to the tip surface of the spray nozzle is preferably 100 mm or more, so that even when oligomers are deposited on the exhaust mechanism, it is difficult to fall on the film.
- the inter-nozzle exhaust mechanism 4 is completely separated from the spray nozzle 6, installed on the back surface of the spray nozzle, and a gap is provided between the spray nozzles.
- the air that is sprayed and rebounds on the film surface passes through the gap between the spray nozzles and is sucked into the exhaust on the back surface of the nozzle.
- “completely separated” means that all the spray nozzles are not in contact with the suction surface as shown in FIG. 3, while FIG. 1 shows that the spray nozzle 6 and the inter-nozzle exhaust mechanism 4 are separated. There is no example. Simply, separation refers to the case where at least one of the spray nozzles of FIG. 1 is not in contact with the suction surface as in the spray nozzle of FIG.
- the spray nozzle closest to the extrusion die that is, the topmost spray nozzle
- the spray air acts as a curtain and has the effect of suppressing the blow-up.
- the inclination angle of the uppermost spray nozzle is preferably 0 to 20 ° in the direction of rotation of the cooling drum, and if it is further inclined, the cooling efficiency at the uppermost stage is lowered.
- the defect portion was lightly wiped using Kimwipe (registered trademark) infiltrated with methyl ethyl ketone, and it was confirmed that the defect portion did not disappear so that it was not a foreign matter derived from the coating layer.
- the film sample in which the continuous use time of the cooling device has elapsed for 24 hours was observed from the anti-cooling drum surface.
- Evaluation B Air in the vicinity of the spray nozzle blows toward the extrusion die, but does not reach the position immediately below the extrusion die. Although the air from the spray nozzle hits the film slightly obliquely and the cooling efficiency is slightly lowered, the oligomer in the vicinity of the die does not flow into the cooling device, which is preferable.
- Evaluation C The air in the vicinity of the spray nozzle is almost retained and no wind is generated, or suction and blowing are repeated at random. The air from the spray nozzle hits the film straightly, so that the cooling efficiency is high, and the oligomer in the vicinity of the base does not flow into the inside of the cooling device, which is most preferable.
- Evaluation D Air in the vicinity of the spray nozzle is gently sucked in the rotation direction of the cooling drum. In addition to the fact that the air from the spray nozzle strikes the film slightly obliquely and the cooling efficiency is slightly lowered, air having a high oligomer concentration in the vicinity of the base flows into the cooling device, which is not preferable.
- Evaluation E Air in the vicinity of the spray nozzle is vigorously sucked in the rotation direction of the cooling drum. In addition to the fact that the air from the spray nozzle strikes the film obliquely and the cooling efficiency is lowered, air having a high oligomer concentration in the vicinity of the base flows into the cooling device, which is not preferable.
- Cleanliness of casting chamber The cleanness of the casting chamber was measured using a particle counter. The measurement was performed at two positions, a position directly above the cooling drum and a position directly above the uppermost spray nozzle of the cooling device, and the average value was used as an index of cleanliness. Regarding the suitability as an optical application, from the evaluation results of the films described above, the film satisfies all the conditions that the surface foreign matter defects are 5 pieces / m 2 or less, the crystallization scratches are 5 pieces / m 2 or less, and the thickness unevenness R is 10 ⁇ m or less. Was passed.
- Example 1 Polyethylene terephthalate resin (Toray Co., Ltd., F20S) pellets were dried under reduced pressure as a polyester raw material, then supplied to an extruder and melt extruded at 280 ° C. This was closely adhered to a cooling drum (diameter ⁇ 1600 mm) maintained at a surface temperature of 20 ° C. by an electrostatic application method, and simultaneously cooled and solidified using the present cooling device to obtain a thermoplastic resin film having a thickness of 2100 ⁇ m.
- a cooling drum diameter ⁇ 1600 mm
- a first spray nozzle is disposed at a portion closest to the extrusion die from which the thermoplastic resin is extruded, and the exhaust mechanism between the nozzles is completely separated from the spray nozzle, and 50 mm away from the back surface of the spray nozzle. Installed. Therefore, the suction surface of the inter-nozzle exhaust mechanism is completely separated from the tip surface of the spray nozzle, and there is a gap between the spray nozzles.
- the spray nozzles are installed in 15 stages at a pitch of 100 mm along the rotation direction of the cooling drum, and there is a gap between the spray nozzles, so that air that bounces off against the film passes.
- the part from which air blows is a slit type, and has a slit gap of 2 mm and a width of 1400 mm.
- the suction surface of the inter-nozzle exhaust mechanism is provided with a blind type shielding plate, and the exhaust amount can be varied by adjusting the opening degree.
- the length along the rotation direction of the cooling drum from directly above the top of the cooling drum to the point where the blowing air of the first blowing nozzle arrives is 1400 mm.
- the rotation speed of the cooling drum was 8 m / min
- the total blowing air volume was 90 m 3 / min
- the total suction air volume of the exhaust mechanism between nozzles was 70 m 3 / min
- the cooling air temperature was 11 ° C.
- the cooling drum and the main cooling device are in a space partitioned by a cover or the like as one room (hereinafter referred to as a casting room), have a floor of 5 m square, a ceiling height of 5 m, and a volume of 125 m 3 .
- the casting chamber is provided with an exhaust mechanism around the extrusion die on the ceiling, the ventilation frequency is 80 times / hr, and the indoor cleanliness is class 1000.
- thermoplastic resin film was heated with a heated roll group and an infrared heater, and then stretched 3.2 times in the longitudinal direction with a roll group having a peripheral speed difference to obtain a uniaxially oriented polyester film. Subsequently, the end of the film was gripped with a clip, led to a hot air zone having a temperature of 130 ° C., and stretched 3.5 times in the film width direction. Next, while maintaining the stretched width, heat fixing treatment is performed in a hot air zone at a temperature of 220 ° C., cooling treatment is further performed in a hot air zone at a temperature of 100 ° C., and both ends of the film are trimmed.
- biaxially oriented polyester film having a thickness of 188 ⁇ m and a width of 3450 mm was obtained.
- the obtained biaxially oriented polyester film was removed by 150 mm from both ends, and divided into three portions of 1000 mm width and slitted to obtain three polyester film rolls having a width of 1000 mm and a length of 2000 m. Of these three, a central roll was used to produce a film roll sample required for evaluation of thickness unevenness, surface foreign matter, crystallization scratches, and the like.
- Example 2 In this cooling device, there is a suction surface of the inter-nozzle exhaust mechanism between each spray nozzle, and the distance from the front end surface of the spray nozzle to the suction surface of the inter-nozzle exhaust mechanism is 100 mm. Therefore, the inter-nozzle exhaust mechanism is not separated from the spray nozzle, and there is no gap between the spray nozzles.
- Example 2 Other than that was carried out similarly to Example 1, and obtained the polyester film roll of thickness 188 micrometers, width 1000mm, and length 2000m.
- Example 4 In the cooling process conditions, the cooling air temperature was 15 ° C. Further, the inter-nozzle exhaust mechanism was separated from the spray nozzle, installed on the back surface of the spray nozzle, and a gap was provided between the spray nozzles. Other than that was carried out similarly to Example 1, and obtained the polyester film roll of thickness 188 micrometers, width 1000mm, and length 2000m. (Example 5) Under the cooling process conditions, a polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m was obtained under the same conditions as in Example 1 except that no ceiling exhaust was installed. The cleanliness in the casting room is class 3000.
- a suction surface is arranged at a portion closest to the extrusion die, a suction surface of a nozzle exhaust mechanism is disposed between each spray nozzle and the spray nozzle, and a tip surface of the spray nozzle and an exhaust mechanism between the nozzles
- the suction surfaces were placed on the same circumference. Therefore, no gap is provided between the spray nozzles.
- a heater was placed on the wall inside the suction surface as a measure to prevent oligomer precipitation on the suction surface.
- the length along the rotation direction of the cooling drum from directly above the top of the cooling drum to the landing point of the blowing air of the first blowing nozzle was set to 1400 mm.
- the total blowing air volume was 90 m 3 / min, the total suction air volume was 340 m 3 / min, and the total suction air volume / total blowing air volume was 3.78.
- Conditions other than these were the same as in Example 1 to obtain a polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m.
- Comparative Example 3 A polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m was obtained in the same manner as in Comparative Example 1 except that the number of evoke in the casting chamber was 120 times / Hr. The cleanliness in the casting room is class 800.
- Comparative Example 4 A polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m was obtained in the same manner as in Comparative Example 1 except that the distance from the tip surface of the spray nozzle to the suction surface of the inter-nozzle exhaust mechanism was set to 100 mm.
- Comparative Example 5 A first spray nozzle was installed in the part closest to the extrusion die. Further, no heater is installed inside the first suction surface. Conditions other than these were the same as in Comparative Example 1 to obtain a polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m.
- Comparative Example 6 A first spray nozzle was installed in the part closest to the extrusion die. Further, no heater is installed inside the first suction surface. Further, the suction surface of the inter-nozzle exhaust mechanism is separated from the tip surface of the spray nozzle. Conditions other than these were the same as in Comparative Example 1 to obtain a polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m.
- Comparative Example 7 A first spray nozzle was installed in the part closest to the extrusion die. Further, no heater is installed inside the first suction surface. A polyester film roll having a thickness of 188 ⁇ m, a width of 1000 mm, and a length of 2000 m was obtained in the same manner as in Comparative Example 1 except that the distance from the tip surface of the spray nozzle to the suction surface of the inter-nozzle exhaust mechanism was 100 mm. It was.
- the film obtained by the production method and production apparatus of the present invention has excellent optical characteristics, and it has been difficult to achieve compatibility with conventional film production techniques with large thickness unevenness. It is suitable for display related applications.
- Extrusion die 2 Cooling drum 3: Thermoplastic resin film 4: Exhaust mechanism between nozzles 5: Exhaust die peripheral exhaust mechanism 6: Spray nozzle 7: Separating roll 8: Suction surface of inter-nozzle exhaust mechanism 9: Tip of spray nozzle Surface 10: Length along the rotation direction of the cooling drum from directly above the top of the cooling drum to the landing point of the blowing air of the first blowing nozzle 11: Distance from the suction surface of the exhaust mechanism to the tip surface of the blowing nozzle
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Abstract
Description
こういった問題に対し、溶融させた熱可塑性樹脂を、冷却ドラム上にキャストし、該冷却ドラム上で冷却固化して熱可塑性樹脂フィルムを形成するに際し、該フィルムの反冷却ドラム面からフィルムに向けて、前期冷却ドラムの幅方向に延びる吹き付けノズルを含む給気手段により冷却用空気を吹き付けつつ、複数の排気孔が穿設された遮閉板を含むノズル間排気機構により、フィルム近傍の空気を吸引、排出し、かつ、この給気と排気手段をフィルム流れ方向に交互に行うことを特徴とする熱可塑性樹脂フィルムの製造方法が知られている(例えば、特許文献2)。
(1)フィルム厚みムラ
長さ1m、幅600mmのフィルムサンプルから、フィルムサンプルの幅方向中心部および端部から100mmの位置をサンプル中央とするようにして、幅40mmの厚み測定用サンプルを3箇所切り出した。その後、接触式厚み計(アンリツ(株)製KG60/A)を用いて、各厚み測定用サンプルの長手方向の厚みを連続的に測定してチャートレコーダに出力した。出力した厚みのプロファイルから厚みの最大値(MAX)と最小値(MIN)の差を厚みムラR(=MAX-MIN)μmとした。厚みムラRは3箇所の値を平均したものとする。
長さ1m、幅600mmのフィルムサンプルを暗室内で垂直方向に垂らし、フィルム背面の全面に光沢の無い黒色の布を配置し、配向フィルムを巻き出しつつ、前面(被覆層面)からブロムライトを用いてフィルム面に対し約10°から45°の範囲で該ブロムライトの角度を変えながら、フィルム正面から観察し、長径0.5mm以上の異物欠点をマーキングし、フィルム面積1m2当たりの欠点個数を数えた。そのさい、メチルエチルケトンを浸透させたキムワイプ(登録商標)を用いて欠点部を軽く拭き、欠点部が消失しないことで塗布層由来の異物でないことを確認した。なお、表面異物欠点は製膜時間の経過とともに増加するため、本冷却装置の連続使用時間が24Hr経過したフィルムサンプルに対して反冷却ドラム面から観察した。
長さ1m、幅600mmのフィルムサンプルについて、フィルムサンプルを暗室内で垂直方向に垂らし、反冷却ドラム面から3波長蛍光灯(パナソニック(株)パルック3波長形昼白色(F.L 15EX-N 15W))の投光器反射で10mmを越えるキズをマーキングし、マーキングしたキズに対して光学顕微鏡(倍率400倍)で測定し、複数の突起物が集中して10mmを越える形状となっているキズを結晶化キズとして数えた。
JIS-K7105(1981)にもとづき、ヘイズメーター(「NDH2000」、日本電色工業(株)製)を用いて測定した。長さ1m、幅600mmのフィルムサンプルに対して、長さ方向、幅方向の一辺が100mmの正方形の範囲で、但し、隣り合う正方形同士は重ならず、隣り合う正方形同士が一辺を共有するように、長さ方向9個所×幅方向5個所の計45箇所で測定し、その平均値をとった。
本冷却装置について、第1吹き付けノズルの表面(フィルム幅方向の中央部付近)に長さ50mm、幅50mmのテフロン(登録商標)コーティングを実施したSUS板を取り付けた。本冷却装置の連続使用時間24Hr後、SUS板を吹き付けノズルから取り外し、表面に析出、堆積したオリゴマをメタノール中で洗浄した。その濾液を、分光光度計にセットし、波長240nmの吸光度を測定した。
オリゴマ量の定量化には、あらかじめ吸光度(240nm)とオリゴマ濃度(ppm)の検量線を作成し、吸光度からオリゴマ濃度を推算した。
本冷却装置の第1吹き付けノズル及び前記押出ダイ直下(冷却ドラムの頂点付近)付近に、純水ミスト気流可視化装置(日本エアーテック株式会社 CLEAN VIEWER ACV-501)のホースを向け、可視化装置からの白煙の流れを目視観察した。本冷却装置付近のエアの強さ、向きの状態について、下記のように評価付けした。
評価A:吹き付けノズル付近のエアが押出ダイ直下に向かって勢いよく吹出している。押出ダイから吐出される熱可塑性樹脂がエアによって振動することに加え、吹き付けノズルからのエアが斜めにフィルムに当たっており冷却効率が低下するため、好ましくない。
評価B:吹き付けノズル付近のエアが押出ダイに向かって吹出しているが、押出ダイ直下までは届かない。吹き付けノズルからのエアがフィルムにやや斜めに当たっており冷却効率が若干落ちるが、口金付近のオリゴマが本冷却装置内部へ流入しておらず好ましい。
評価C:吹き付けノズル付近のエアがほとんど滞留して無風、あるいは吸込みと吹出しをランダムに繰り返している。吹き付けノズルからのエアがフィルムにまっすぐ当たっており冷却効率が高く、口金付近のオリゴマが本冷却装置内部へ流入しておらず最も好ましい。
評価D:吹き付けノズル付近のエアが緩やかに冷却ドラムの回転方向に吸込まれている。吹き付けノズルからのエアがフィルムにやや斜めに当たっており冷却効率が若干落ちることにくわえ、口金付近のオリゴマ濃度が高いエアが本冷却装置内部へ流入しており好ましくない。
評価E:吹き付けノズル付近の空気が勢いよく冷却ドラムの回転方向に吸込まれている。吹き付けノズルからのエアがフィルムに斜めに当たっており冷却効率が落ちることにくわえ、口金付近のオリゴマ濃度が高いエアが本冷却装置内部へ流入しており好ましくない。
パーティクルカウンタを用いてキャスティング室内のクリーン度を測定した。測定箇所は冷却ドラムの真上の位置および本冷却装置最上段吹き付けノズルの真上の位置の2箇所で行い、その平均値をクリーン度の指標とした。光学用途としての適合性について、前記したフィルムの評価結果から、表面異物欠点が5個/m2以下、結晶化キズ5個/m2以下、厚みムラR=10μm以下の条件をすべて満足するフィルムを合格とした。
ポリエステル原料として、ポリエチレンテレフタレート樹脂(東レ(株)、F20S)ペレットを減圧乾燥した後、押し出し機に供給し、280℃で溶融押出しした。これを表面温度20℃に保った冷却ドラム(直径φ1600mm)に静電印加法にて密着させると同時に、本冷却装置を用いて冷却固化し、厚さ2100μmの熱可塑性樹脂フィルムを得た。
本冷却装置は、熱可塑性樹脂が押出される押出ダイに一番近い部分には、第一吹き付けノズルが配置され、ノズル間排気機構を吹き付けノズルと完全に分離し、吹き付けノズルの背面から50mm離れて設置した。従って、ノズル間排気機構の吸引面は吹き付けノズルの先端面から完全に離れており、吹き付けノズル間には隙間がある。
吹き付けノズルは冷却ドラムの回転方向に沿って100mmピッチで15段設置しており、吹き付けノズルの間には隙間があり、フィルムに当たってはね返ってくるエアが通る。
また、エアが吹き出る部分はスリットタイプとなっていて、スリット間隙2mm、幅1400mmである。
冷却固化の工程条件としては冷却ドラムの回転速度を8m/min、全吹き付け風量を90m 3/min、ノズル間排気機構の全吸引風量を70m3/min、冷却エア温度を11℃とした。
冷却ドラム、本冷却装置は一つの部屋として、カバーなどで仕切られた空間にあり(以下、キャスティング室とする)、床5m四方、天井高さ5mで容積125m3である。キャスティング室には押出ダイ周辺排気機構を天井に設けてあり、換気回数80回/hr、室内のクリーン度はクラス1000である。
本冷却装置において、各々の吹き付けノズルと吹き付けノズルの間にノズル間排気機構の吸引面があり、吹き付けノズルの先端面からノズル間排気機構の吸引面までの距離を100mmとした。従って、ノズル間排気機構は吹き付けノズルと分離しておらず、吹き付けノズル間に隙間はない。それ以外は実施例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
冷却工程条件において、全吹き付け風量を120m3/min、全吸引風量を70m3/min、全吸引風量/全吹き付け風量=0.58とした。また、ノズル間排気機構を、吹き付けノズルと分離し、吹き付けノズルの背面に設置、吹き付けノズル間に隙間を設けた。そして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
冷却工程条件において、冷却エア温度を15℃とした。また、ノズル間排気機構を、吹き付けノズルと分離し、吹き付けノズルの背面に設置、吹き付けノズル間に隙間を設けた。それ以外は実施例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
(実施例5)
冷却工程条件において、天井排気を設置しない以外は実施例1と同様の条件にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。なお、キャスティング室内のクリーン度はクラス3000である。
冷却工程条件において、全吹き付け風量を90m3/min、全吸引風量を90m3/min、全吸引風量/全吹き付け風量=1.00とした。また、ノズル間排気機構を、吹き付けノズルと分離し、吹き付けノズルの背面に設置、吹き付けノズル間に隙間を設けた。それ以外は実施例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
冷却工程条件において、全吹き付け風量を90m3/min、全吸引風量を45m3/min、全吸引風量/全吹き付け風量=0.50とした。また、天井排気を設置していない。また、ノズル間排気機構を、吹き付けノズルと分離し、吹き付けノズルの背面に設置、吹き付けノズル間に隙間を設けた。それ以外は実施例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
(実施例8)
冷却工程条件において、全吹き付け風量を90m3/min、全吸引風量を81m3/min、全吸引風量/全吹き付け風量=0.90とした。また、天井排気を設置していない。また、ノズル間排気機構を、吹き付けノズルと分離し、吹き付けノズルの背面に設置、吹き付けノズル間に隙間を設けた。それ以外は実施例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
本冷却装置において、押出ダイに一番近い部分に吸引面を配置し、各々の吹き付けノズルと吹き付けノズルの間にはノズル排気機構の吸引面を配置し、吹き付けノズルの先端面とノズル間排気機構の吸引面の位置は同じ円周上に配置した。従って、吹き付けノズル間に隙間は設けない。また、吸引面へのオリゴマ析出防止対策として、吸引面内部の壁面にヒーターを配置した。
また、冷却ドラムの頂点真上から第一吹き付けノズルの吹き付けエアの着地点までの冷却ドラムの回転方向に沿った長さを1400mmとした。また、全吹き付け風量90m3/min、全吸引風量を340m3/minとし、全吸引風量/全吹き付け風量=3.78とした。これら以外の条件は実施例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
全吹き出し風量を90m3、全吸引風量を225m3/minとし、全吸引風量/全吹き付け風量=2.50とした以外は比較例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
キャスティング室内の喚起回数を120回/Hrとした以外は比較例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。なお、キャスティング室内のクリーン度はクラス800である。
吹き付けノズルの先端面からノズル間排気機構の吸引面までの距離を100mmに離した以外は比較例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
押出ダイに一番近い部分に第1吹き付けノズルを設置した。また、第1吸引面の内部にはヒーターを設置していない。これら以外の条件は比較例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
押出ダイに一番近い部分に第1吹き付けノズルを設置した。また、第1吸引面の内部にはヒーターを設置していない。また、ノズル間排気機構の吸引面は吹き付けノズルの先端面から離れている。これら以外の条件は比較例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
押出ダイに一番近い部分に第1吹き付けノズルを設置した。また、第1吸引面の内部にはヒーターを設置していない。また、吹き付けノズルの先端面からノズル間排気機構の吸引面までの距離を100mmとした以外の条件は比較例1と同様にして、厚さ188μm、幅1000mm、長さ2000mのポリエステルフィルムロールを得た。
2:冷却ドラム
3:熱可塑性樹脂フィルム
4:ノズル間排気機構
5:押出ダイ周辺排気機構
6:吹き付けノズル
7:引き離しロール
8:ノズル間排気機構の吸引面
9:吹き付けノズルの先端面
10:冷却ドラムの頂点真上から第一吹き付けノズルの吹き付けエアの着地点までの冷却ドラムの回転方向に沿った長さ
11:排気機構の吸引面から吹き付けノズルの先端面までの距離
Claims (6)
- 溶融させた熱可塑性樹脂を押出ダイより冷却ドラム上にキャストし、該冷却ドラム上で冷却固化して熱可塑性樹脂フィルムを製造するに際し、冷却ドラムに接しないフィルム面(以下、反冷却ドラム面とする)から吹き付けノズルでフィルムに向けてエアを吹き付けながら、同時に反冷却ドラム面からノズル間排気機構でフィルム近傍のエアを吸引する装置であって、該ノズル間排気機構の吸引面が、該吹き付けノズルの先端面よりフィルムから離れた位置に設置されたことを特徴とする熱可塑性樹脂フィルムの製造装置。
- ノズル間排気機構を、吹き付けノズルと分離して、吹き付けノズルの背面に設置し、吹き付けノズル間に隙間を設ける請求項1に記載の熱可塑性樹脂フィルムの製造装置。
- 吹き付けるエアの単位時間当たりの総量をS、吸引するエアの単位時間当たりの総量をEとした時、SがEより大きいかまたは等しい請求項1または2に記載の熱可塑性樹脂フィルムの製造装置。
- 前記吹き付けノズルの内、押出ダイの最も近くに位置する吹き付けノズルが、フィルム面に対して角度調整が可能な角度調整機構を有することを特徴とする請求項1~3のいずれかに記載の熱可塑性樹脂フィルムの製造装置。
- 溶融させた熱可塑性樹脂を押出ダイより冷却ドラム上にキャストし、該冷却ドラム上で冷却固化して熱可塑性樹脂フィルムを製造するに際し、冷却ドラムに接しないフィルム面(以下、反冷却ドラム面とする)からフィルムに向けてエアを吹き付けながら、同時に反冷却ドラム面からフィルム近傍のエアを吸引する工程を有する熱可塑性樹脂フィルムの製造方法であって、吹き付けるエアの単位時間当たりの総量をS、吸引するエアの単位時間当たりの総量をEとした時、SがEより大きいかまたは等しいことを特徴とする熱可塑性樹脂フィルムの製造方法。
- 前記E/Sの比率が0.5~0.9の範囲である請求項5に記載の熱可塑性樹脂フィルムの製造方法。
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US (1) | US9266273B2 (ja) |
EP (1) | EP2487023B1 (ja) |
JP (1) | JP5799505B2 (ja) |
KR (1) | KR101791487B1 (ja) |
CN (1) | CN102574320B (ja) |
MY (1) | MY175152A (ja) |
TW (1) | TWI558535B (ja) |
WO (1) | WO2011043285A1 (ja) |
Cited By (2)
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---|---|---|---|---|
JP2014061671A (ja) * | 2012-09-24 | 2014-04-10 | Mitsubishi Plastics Inc | ポリエステルシートの製造方法 |
CN117405677A (zh) * | 2023-12-14 | 2024-01-16 | 常州树杰塑业有限公司 | 一种塑料薄膜裂缝检测装置 |
Families Citing this family (1)
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---|---|---|---|---|
CN110605801B (zh) * | 2019-09-18 | 2021-08-03 | 安徽冠泓塑业有限公司 | 一种塑料流延工艺辅助冷却设备 |
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- 2010-10-04 EP EP10821955.1A patent/EP2487023B1/en active Active
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- 2010-10-04 US US13/500,819 patent/US9266273B2/en active Active
- 2010-10-04 MY MYPI2012001536A patent/MY175152A/en unknown
- 2010-10-04 KR KR1020127006367A patent/KR101791487B1/ko active IP Right Grant
- 2010-10-04 WO PCT/JP2010/067348 patent/WO2011043285A1/ja active Application Filing
- 2010-10-04 JP JP2010547886A patent/JP5799505B2/ja active Active
- 2010-10-06 TW TW099134022A patent/TWI558535B/zh not_active IP Right Cessation
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2014061671A (ja) * | 2012-09-24 | 2014-04-10 | Mitsubishi Plastics Inc | ポリエステルシートの製造方法 |
CN117405677A (zh) * | 2023-12-14 | 2024-01-16 | 常州树杰塑业有限公司 | 一种塑料薄膜裂缝检测装置 |
CN117405677B (zh) * | 2023-12-14 | 2024-03-22 | 常州树杰塑业有限公司 | 一种塑料薄膜裂缝检测装置 |
Also Published As
Publication number | Publication date |
---|---|
TWI558535B (zh) | 2016-11-21 |
KR101791487B1 (ko) | 2017-10-30 |
JPWO2011043285A1 (ja) | 2013-03-04 |
EP2487023A1 (en) | 2012-08-15 |
US9266273B2 (en) | 2016-02-23 |
TW201117944A (en) | 2011-06-01 |
EP2487023A4 (en) | 2014-12-10 |
US20120200002A1 (en) | 2012-08-09 |
MY175152A (en) | 2020-06-11 |
CN102574320A (zh) | 2012-07-11 |
KR20120096464A (ko) | 2012-08-30 |
EP2487023B1 (en) | 2017-04-19 |
CN102574320B (zh) | 2015-12-02 |
JP5799505B2 (ja) | 2015-10-28 |
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