WO2015047014A1 - Pellicule anti-adhésive et son procédé de fabrication - Google Patents

Pellicule anti-adhésive et son procédé de fabrication Download PDF

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Publication number
WO2015047014A1
WO2015047014A1 PCT/KR2014/009170 KR2014009170W WO2015047014A1 WO 2015047014 A1 WO2015047014 A1 WO 2015047014A1 KR 2014009170 W KR2014009170 W KR 2014009170W WO 2015047014 A1 WO2015047014 A1 WO 2015047014A1
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Prior art keywords
release
film
formula
particles
release film
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PCT/KR2014/009170
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English (en)
Korean (ko)
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임미소
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코오롱인더스트리 주식회사
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Priority claimed from KR1020140130362A external-priority patent/KR102204965B1/ko
Application filed by 코오롱인더스트리 주식회사 filed Critical 코오롱인더스트리 주식회사
Priority to JP2016517544A priority Critical patent/JP6165326B2/ja
Priority to CN201480052866.5A priority patent/CN105637042B/zh
Priority to EP14849767.0A priority patent/EP3053969A4/fr
Priority to US15/025,712 priority patent/US20160237287A1/en
Publication of WO2015047014A1 publication Critical patent/WO2015047014A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
    • C09D183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/0427—Coating with only one layer of a composition containing a polymer binder
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/043—Improving the adhesiveness of the coatings per se, e.g. forming primers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/04—Coating
    • C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C09J7/405—Adhesives in the form of films or foils characterised by release liners characterised by the substrate of the release liner
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2467/00—Presence of polyester
    • C09J2467/006—Presence of polyester in the substrate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2483/00—Presence of polysiloxane
    • C09J2483/005—Presence of polysiloxane in the release coating

Definitions

  • the present invention relates to a release film. More specifically, the present invention relates to an in-line coating release film used for electronic materials such as ceramic multilayer capacitors (MLCC), polarizing plate protection, and OCA.
  • MLCC ceramic multilayer capacitors
  • OCA polarizing plate protection
  • Polyester film has excellent physical stability in a wide temperature range from low temperature to high temperature, and excellent chemical resistance compared to other polymer resins.
  • the mechanical strength, surface properties and uniformity of the thickness is good, it can be applied to various applications or process conditions. Therefore, it is applied to a capacitor, a photo film, a label, a pressure-sensitive tape, a decorative laminate, a transfer tape, a polarizing plate, and a green sheet for releasing ceramics, and in recent years, the demand is increasing in response to the trend of high speed and automation.
  • the film for electronic materials has recently been intensifying competition with the downturn in the optical market, requiring a higher level of physical properties and cost reduction.
  • Polyester film for ceramic capacitor green sheet molding is used as a release film by coating another polymer resin on the base film.
  • the release film is produced, the characteristics of running, adhesion, uniform surface shape, transparency, etc. are required.
  • the modification of the base film itself, as well as the method of improving the silicone coating bath solution has emerged as an important requirement.
  • the uniform surface shape of the base film becomes an important base film requirement.
  • Korean Laid-Open Patent Publication No. 2003-0055118 shows that when the ceramic slurry is applied on a release film, pinhole formation of the ceramic slurry layer is greatly suppressed and also when providing a ceramic layer on the release film. Since the rate of change of the thickness of the ceramic layer is lowered, it is possible to give excellent release performance and provide a polyester film useful as a substrate of the release film.
  • the maximum protrusion height (Rmax) at one side (surface A) of the polyester film is 500 nm or less.
  • a polyester film for a release film having a thickness change rate of 5% or less which is defined by the following formula using the maximum, minimum and average values of the film thickness in the longitudinal and transverse directions of the polyester film.
  • the release film which contains a release layer in one side of such a polyester film.
  • Korean Laid-Open Patent Publication No. 1999-0088139 (1999.12.27) provides a release film that does not block even when a release film having a flat release layer surface is rolled onto a roll, and is suitable for forming a thin film green sheet.
  • the center line average roughness Ra of the surface of the release layer is 30 nm or less
  • a distribution curve showing the relationship between the protrusion height (X) and the number of protrusions (Y) on the surface of the release layer has a protrusion height of 0.05 to 0.3 ⁇ m. It is characterized by satisfy
  • the present invention provides a polyester film that has a smooth surface and can be used as a base film suitable for a release film for electronic materials, and to manufacture a release film using the same.
  • the present invention has a maximum acid height surface roughness (Rp) of 0.27 ⁇ m or less on one side of the film (surface A) is good, preferably 0.1 ⁇ m to 0.27 ⁇ m, the size of the defect is reduced, polyester excellent in workability To provide a film.
  • Rp maximum acid height surface roughness
  • the present invention is the polyester film as a base film, by forming a release coating layer on one side or both sides of the base film is excellent in adhesive strength with the polyester film, less change and variation over time of release force, To provide a release film having a high residual adhesion rate.
  • the present invention is to provide a release film which is a thin film with a thickness of the polyester base film 10 ⁇ 50 ⁇ m. Accordingly, the coating thickness of the release layer is also 0.07 ⁇ 0.3 ⁇ m to provide a coating composition for release coating that can be coated by an in-line coating method so that it can be coated with a thin film and a method for producing a release film using the same.
  • the present invention solves the problem that the release coating layer is unevenly coated during coating by the in-line coating method, to form a uniform coating layer as the surface roughness of the polyester base film is lowered, winding property and fish eye generation To provide a release film that does not.
  • the present invention for achieving the above object is a polyester base film comprising particles satisfying the following formula 1 to formula 3,
  • the release force change rate includes a release film comprising a release coating layer satisfying the following formula 4, the release force deviation satisfies the following formula 5.
  • Pa is the average particle diameter ( ⁇ m) of the particles
  • Dmax means the maximum particle diameter ( ⁇ m) of the particles.
  • R i is the release force measured after standing at 55 ° C. for 24 hours
  • R f is the release force measured after standing at 55 ° C. for 240 hours.
  • R f-max is the maximum value of the release force measured five times after standing at 55 °C for 240 hours
  • Pa is the average particle diameter ( ⁇ m) of the particles
  • Dmax means the maximum particle diameter ( ⁇ m) of the particles.
  • It relates to a method for producing a release film comprising a.
  • n is from 20 to 3000, m is from 1 to 500, and n + m is from 21 to 3000.
  • the release film according to the present invention effectively controls the maximum particle diameter (Dmax) for the average particle diameter and particle size distribution of the particles, thereby satisfying the surface properties that a high smooth release film for ceramic multilayer capacitors (MLCC) should have basically, polarizing plate It has high smooth surface characteristics required for application to electronic materials such as protective or OCA. In addition, it is possible to effectively control the generation of pinholes by controlling the appropriate surface roughness to secure the winding and workability, and to reduce the fish eye.
  • Dmax maximum particle diameter
  • MLCC ceramic multilayer capacitors
  • the release film according to the present invention is suitable for use in electronic materials without blocking occurs even when the release layer surface is flat and wound onto a roll.
  • the release film according to the present invention is coated by the in-line coating method can reduce the loss caused by the post-processing, can reduce the processing process, there is a cost saving effect.
  • the release film according to the present invention is coated by the in-line coating method can reduce the loss caused by the post-processing, can reduce the processing process, there is a cost saving effect.
  • by forming a uniform coating layer has little change over time and the deviation of the release force, there is an advantage that can achieve excellent release properties with a residual adhesion of 90% or more.
  • the manufacturing method of the release film according to the present invention has the advantage of maximizing the product properties through controlling the surface characteristics of the base film and reducing the cost by introducing an inline coating process, thereby maximizing economical and productivity.
  • 1 is a graph showing the position of the maximum particle diameter in the present invention.
  • the particles may be added when the polyester resin is synthesized, or may be mixed in the melt extrusion step after the polyester resin is synthesized.
  • a slurry state ie, particles and glycol
  • One aspect of the present invention is a polyester base film containing particles satisfying the following formulas (1) to (3).
  • Pa is the average particle diameter ( ⁇ m) of the particles
  • Dmax means the maximum particle diameter ( ⁇ m) of the particles.
  • the maximum particle size of the particles when the maximum particle size of the particles is less than 0.6 ⁇ m, the surface smoothness of the polyester base film is improved, but scratches or winding properties due to friction in the film manufacturing process may be poor projections and foam outage may occur have.
  • the maximum particle size of the particles is more than 2.5 ⁇ m, the running and winding properties are excellent, but coarse particles are present, so the probability of defects is increased when manufacturing the polyester base film, and the film surface is stored for a long time by winding with a roll.
  • Orange Peel which looks bumpy like this orange peel, can occur. This causes a coating non-uniformity in the post-process, and has a problem in that it is transferred to a coated pressure-sensitive adhesive or the like to cause a defect.
  • the maximum particle diameter (mu m) of the particles is measured using a particle size distribution analyzer. In this case, it means the size of the particles remaining on the particle size distribution graph immediately before the volume becomes 0%.
  • 1 is a graph showing the particle size distribution of mainly used inorganic particles. Dmax in Fig. 1 means the maximum particle diameter ( ⁇ m).
  • the content of particles is preferably used 0.03 to 0.25% by weight of the total weight of the film.
  • it is used at less than 0.03% by weight, it is difficult to secure runability and mold release property because of the small amount of particles, and a high possibility of winding failure occurs.
  • the maximum acid height surface roughness (Rp) increases to increase the possibility of occurrence of pinholes or fish-eye due to particle aggregation.
  • Equation 3 regarding the correlation between the average particle diameter and the maximum particle diameter, it is preferable to use a particle having a small difference between the average particle diameter and the maximum particle diameter. More preferably, as shown in the particle size distribution graph, a narrow graph containing a large amount of uniform particles may reduce the maximum acid height surface roughness (Rp) to suppress the generation of pinholes.
  • the smoothness is most excellent in the range of Pa / Dmax of 0.1 to 0.4, more preferably 0.2 to 0.38.
  • the particles are preferably added in the form of a slurry dispersed in a glycol when the polyester resin is synthesized, so that the particles are excellent in dispersibility and can prevent reaggregation between the particles, and the present invention is not limited thereto.
  • the polyester may be obtained by condensation polymerization of an acid component containing dicarboxylic acid as a main component and a glycol component containing alkyl glycol as a main component, and particles may be added in the condensation polymerization step or a solid phase polymerization step. It is preferable to throw in the slurry state disperse
  • the polyester resin constituting the polyester base film may be a resin obtained by condensation polymerization of an acid component containing dicarboxylic acid as a main component and a glycol component containing alkyl glycol as a main component.
  • Terephthalic acid or its alkyl ester or phenyl ester is mainly used as the main component of the dicarboxylic acid, but a part thereof is used, for example, isophthalic acid, oxyethoxy benzoic acid, adipic acid, sebacic acid, and 5-sodium sulfoisophthalic acid. It may be used in place of a bifunctional carboxylic acid or an ester forming derivative thereof.
  • ethylene glycol is the main object, but a part thereof is propylene glycol, trimethylene glycol, 1,4-cyclohexanediol, 1,4-cyclohexanedimethanol, 1,4-bisoxyethoxy It can also be used by replacing with benzene, bisphenol, and polyoxyethylene glycol, and if it is a small content, you may use together a monofunctional compound or a trifunctional compound.
  • the particles are not particularly limited as long as the average particle diameter, amount of addition and size distribution are within the scope of the present invention.
  • the average particle size is 0.15 ⁇ 0.6 ⁇ m
  • the amount of added particles is 0.03 ⁇ 0.25% by weight
  • the coarse particles are removed to have a maximum particle size (Dmax) of 0.6 ⁇ 2.5 ⁇ m in the particle size distribution.
  • the kind of particles is not limited, and may be an inorganic particle, an organic particle, or a mixture of inorganic particles and organic particles, and one or two or more kinds thereof may be used. That is, it is also possible to use one or two or more kinds of inorganic particles, one or two or more kinds of organic particles, or use a mixture of one or two or more kinds of inorganic particles and one or two or more kinds of organic particles. Do.
  • the inorganic particles may be calcium carbonate, titanium oxide, silica, kaolin and barium sulfate, and the like, and the organic particles may be silicone resin, crosslinked divinylbenzene polymethacrylate, crosslinked polymethacrylate, crosslinked polystyrene resin, Benzoguanamine-formaldehyde resin, benzoguanamine-melamine-formaldehyde resin, melamine-formaldehyde resin, etc. can be used.
  • the polyester base film may have a haze of 1.5 to 10%.
  • the haze of the film is less than 1.5%, it is excellent in transparency, but the particle content is insufficient to cause a winding defect on the roll.
  • the haze is more than 10%, the transparency is low, the pinholes commonly used in green sheet and film for electronic materials And the inspection of defective parts such as defects.
  • the polyester base film has a maximum acid height surface roughness (Rp) of 0.1 ⁇ 0.27 ⁇ m.
  • the maximum peak height surface roughness (Rp) is based on JIS B0601, using a two-dimensional surface roughness measuring instrument (Kosaka Lab. Surfcorder SE-3300) measuring speed of 0.05mm / sec, the contact radius 2 ⁇ m, load 0.7mN The cutoff value is measured under a condition of 0.08 mm, and a total length of five times is selected from the curve of the cross section of the film in the direction of the center line, and the average value is calculated. At this time, the highest profile peak height from the centerline within the sampling length is taken as the maximum peak height surface roughness Rp.
  • the polyester base film according to the present invention has a maximum acid height surface roughness (Rp) of 0.27 ⁇ m or less, and more preferably, has a maximum acid height surface roughness (Rp) of 0.1 to 0.27 ⁇ m.
  • the polyester base film may have a static friction coefficient and dynamic friction coefficient of 0.2 ⁇ 0.5. If the static friction coefficient and the dynamic friction coefficient are more than 0.5, the coiling property is poor, causing protrusion and scratches, and stable operation is impossible. If it is less than 0.2, the slipperiness
  • the release coating layer of the present invention has a poor winding property as the smoothness of the polyester base film having lowered the surface roughness is improved, and when the release composition is coated, a fish eye occurs or a problem in which the release coating layer is unevenly coated is improved.
  • the present inventors have found that such a problem can be solved by forming a release coating layer satisfying the following Equations 4 and 5, thereby completing the present invention.
  • R i is the release force measured after standing at 55 ° C. for 24 hours
  • R f is the release force measured after standing at 55 ° C. for 240 hours.
  • R f-max is the maximum value of the release force measured five times after standing at 55 °C for 240 hours
  • Equation 4 means the change over time of the release force. As the change over time is less than the final product can be used for long-term storage, there is an advantage of management, it is preferable to exhibit a uniform peeling force when peeling the release film. If the change in the release force over time is less than 25, it is preferable that no trace of peeling is left when the film is peeled off with a width of 1000 mm or more. On the other hand, if the thickness exceeds 25, a high release force may appear when the film is peeled off by 1000 mm or more, and thus, a trace of peeling of the release film may be left on the surface of the green sheet or electronic material sheet.
  • Equation 5 means the release force deviation. If the deviation of the values of the release force measured after leaving at 55 °C for 240 hours is less than 2 can not feel the release force deviation, it is preferable because the noise does not appear during peeling. On the other hand, if it exceeds 2, it may sense the release force sensation sensibly, and noise (peel and peeling) may occur when peeling.
  • the release coating layer of the present invention for expressing the physical properties may be formed to include the compound of Formula 1 and the compound of Formula 2.
  • n is from 20 to 3000, m is from 1 to 500, and n + m is from 21 to 3000.
  • Formula 1 is a prepolymer state as a subject of the release coating layer, and Formula 2 reacts with Formula 1 as a curing agent to form PDMS (Polydimethylsilicone Resin).
  • the vinyl group of formula 1 reacts with the silane group of formula 2, and in formula 2, the random crosslinking of the silane group (Si-H) and Si-CH 3 is more stable than the curing agent in which only Si-H is continuous.
  • the reaction rate is low, it is preferable, because it does not inhibit the physical properties of the polyester base film of the present invention.
  • the release coating layer includes the compound of Formula 1, the compound of Formula 2, a platinum-based catalyst and a silicon-based wetting agent, and a release coating composition having a solid content of 10 to 30 wt% is coated with a thickness of 0.07 to 0.3 ⁇ m. It may be formed.
  • the release force variation occurs due to insufficient coverage of the polyester film surface, and when the content exceeds 30% by weight, the reaction conversion rate of the release coating layer is not sufficient due to insufficient heat supply from the in-line coating. Can be lowered.
  • the coating thickness is less than 0.07 ⁇ m high peaks of the polyester film is not covered with a coating layer, the release force is high, and when the coating thickness is more than 0.3 ⁇ m may cause a coating stain and a reaction conversion rate of the release coating layer.
  • platinum-based catalyst Commercialized examples include Wacker's EM440.
  • silicone-based wetting agent Commercialized examples include Dow Corning's Q2-5212.
  • the release coating composition may have a solid content of 5 to 25% by weight, more specifically 8 to 16% by weight of the compound of Formula 1. If it is less than 5 wt%, the surface of the film may not be sufficiently covered. If it is more than 25 wt%, the reaction conversion rate may be low to increase the residual adhesion rate.
  • Solid content of the compound of Formula 2 may be 0.5 to 5% by weight, more specifically 0.8 to 2% by weight. If less than 0.5% by weight does not sufficiently cure the release coating layer, if more than 5% by weight unreacted Silane Group may remain to increase the change in release force over time.
  • Solid content of the platinum-based catalyst may be 0.001 to 3% by weight, more specifically 0.005 to 0.1% by weight.
  • Solid content of the silicone-based wetting agent may be 0.1 to 3% by weight, more specifically 0.5 to 2% by weight. If it is less than 0.1% by weight, the effect is insignificant, and if it is more than 3% by weight, coating stains may be caused.
  • the release film according to the present invention is maintained for 24 hours at 70 °C in the adhesive tape adhered state, after removing the adhesive tape, and laminated on a Teflon sheet, the residual adhesiveness calculated according to the following formula 6 is 90% or more It may be.
  • Residual adhesion rate adhesive strength of the adhesive tape after aging for 24 hours at 70 °C / adhesive strength of the initial adhesive tape ⁇ 100 (Equation 6)
  • the unreacted material of the release film is low in the range where the residual adhesiveness is 90% or more, it is preferable because the amount of unreacted material of the release film transferred to the final product after the post-processing is less.
  • Pa is the average particle diameter ( ⁇ m) of the particles
  • Dmax means the maximum particle diameter ( ⁇ m) of the particles.
  • n is from 20 to 3000, m is from 1 to 500, and n + m is from 21 to 3000.
  • the release coating composition When the release coating composition is applied in step c) in the manufacturing method of the present invention, it may be applied by using a gravure roll. When using the gravure coating roll, the release coating composition may be applied in a uniform thickness.
  • step d) when the film is less than 130 ° C., breakage of the film occurs, and when it is more than 150 ° C., the uniformity of the film thickness may be deteriorated. In addition, when the stretching ratio is less than 3 times, the film thickness uniformity may be inferior, and when the stretching ratio is more than 4 times, breakage of the film may occur.
  • the heat treatment may be performed at 230 ⁇ 250 °C. Below 230 ° C., the release coating layer may not be sufficiently reacted and may be pushed out. If the release coating layer is above 250 ° C., thermal wrinkles and orange peel of the film may occur.
  • the release film may have a thickness of the polyester base film is 10 ⁇ 50 ⁇ m, the thickness of the release coating layer is 0.07 ⁇ 0.3 ⁇ m.
  • Average particle diameter and maximum particle diameter (Dmax) were measured using a particle size distribution analyzer (Beckman-Coulter, LS13 320). The size of the particles remaining on the particle size graph immediately before the large particles become 0% is called the maximum particle diameter (Dmax). 1 shows a graph of the particle size distribution.
  • the measuring method was measured based on ASTM D-1003, and the polyester film was randomly extracted from 7 parts at 2 sides and 1 center, and then sliced into 5cm x 5cm sized haze measuring instruments (Nihonden Shoku NDH 300A). It was added to the light of 555nm wavelength and calculated by the following equation to calculate the average value except the maximum / minimum value.
  • Haze (%) (total scattered light / total transmitted light) ⁇ 100
  • the largest profile peak height from the centerline within the sampling length was taken as the maximum peak height surface roughness Rp.
  • the area of the part where the release layer is not formed relative to the base film area is 1% or less, and when it exceeds 1%, it is marked as bad.
  • the tape was placed on the release coating layer and rubbed twice with a 2Kg rubber roll and cut into a size of 50 mm x 15 cm to prepare a sample. After the prepared sample was loaded at 70 g / cm 2 and allowed to stand at 55 ° C. for 24 hours, Peel Tester (Chem Instrument, AR-1000) was used to perform 180-degree Peel Peel Evaluation.
  • Peeling speed is 300mm / min. It is measured 5 times and shows the average value.
  • the tape was placed on the release coating layer and rubbed twice with a 2Kg rubber roll and cut into a size of 50 mm x 15 cm to prepare a sample. After the prepared sample was loaded with 70g / cm 2 and left at 55 ° C for 240hr, Peel Tester (Chem Instrument, AR-1000) was used to perform Peel Peel Evaluation of 180 degrees.
  • Peeling speed is 300mm / min. It is measured 5 times and shows the average value.
  • Release time change average Average of 10cm range.
  • Deviation over time variation The difference between the maximum and minimum values is measured while continuously measuring the 10 cm range.
  • the release film is laminated on the adhesive and subjected to a load of 70g / cm 2, left at 55 ° C. for 24hr, and then induces transfer under severe conditions.
  • the adhesive force of the adhesive laminated to Teflon is evaluated.
  • Particle A Calcium carbonate particles having an average particle diameter of 0.59 ⁇ m and a maximum particle diameter ( ⁇ m) of 2.2 ⁇ m
  • Particle B Titanium dioxide particles having an average particle diameter of 0.36 ⁇ m and a maximum particle diameter ( ⁇ m) of 1.52 ⁇ m.
  • Particle C Calcium carbonate particles having an average particle diameter of 0.51 ⁇ m and a maximum particle diameter ( ⁇ m) of 2.42 ⁇ m
  • Particle D Silica particles having an average particle diameter of 0.19 ⁇ m and a maximum particle diameter ( ⁇ m) of 0.6 ⁇ m.
  • Particle E Silica particles having an average particle diameter of 0.34 ⁇ m and a maximum particle diameter ( ⁇ m) of 3.5 ⁇ m.
  • Particle F Silica particles having an average particle diameter of 0.13 ⁇ m and a maximum particle diameter ( ⁇ m) of 1.5 ⁇ m.
  • Coating solution 1 a composition containing 49.99% by weight of polydimethylsiloxane (Wacker, D490) of Formula 1 as a solid content, 0.01% by weight of platinum catalyst (Wacker, EM440) as a solid content, the total solid content is 50% by weight .
  • Coating solution 2 A composition containing 50% by weight of a hydrogen silane compound of formula (Wacker, V-15) as a solid content.
  • Coating solution 3 A composition having a solid content of 80% by weight of a silicone-based wetting agent (Dow Corning, Q2-5212).
  • the polyester chip was melt extruded at 280 ° C., and then rapidly cooled to 24 ° C. using a large roll to obtain a polyester sheet.
  • the obtained polyester sheet was stretched 3.5 times longitudinally at 110 degreeC, and the coating liquid (A) was apply
  • the film After drying and preheating at 150 ° C., the film was stretched 3.5 times in the transverse direction to prepare a biaxially stretched film.
  • the obtained biaxially oriented film was heat treated at 240 ° C. to obtain a polyester film having a thickness of 25 ⁇ m.
  • Example 2 The experiment was performed in the same manner as in Example 1, but the polyester film was prepared by varying the type and content of the particles as shown in Table 1 below.
  • Example 3 is used by mixing Particle A and Particle B
  • Example 6 is used by mixing Particle C and Particle D.
  • silica particle E was used as in Table 1 to prepare a comparative polyester film.
  • a film was prepared in the same manner as in Example 1, except that the coating solution B was used.
  • a film was prepared in the same manner as in Example 2, except that the coating solution C was used.
  • a film was prepared in the same manner as in Example 3, except that the coating solution D was used.
  • silica particle F was used as in Table 1 to prepare a comparative polyester film.
  • the release film according to the present invention has a low surface roughness, was found to be excellent in the initial release force and change over time of the release coating layer, it exhibited a physical property of 90% or more residual adhesion.
  • Comparative Example 5 used the same release coating composition as Example 1, there was a problem in that the film was not wound due to the low surface roughness of 0.0866 (average particle diameter (Pa / Dmax)) of the particles in the film.

Abstract

La présente invention concerne une pellicule anti-adhésive. L'invention concerne plus précisément une pellicule anti-adhésive de revêtement de vernissage en ligne utilisé pour un condensateur céramique multicouche (MLCC), et permettant de protéger une plaque de polarisation, et des matières électroniques pour un OCA et similaire.
PCT/KR2014/009170 2013-09-30 2014-09-30 Pellicule anti-adhésive et son procédé de fabrication WO2015047014A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
JP2016517544A JP6165326B2 (ja) 2013-09-30 2014-09-30 離型フィルムおよびその製造方法
CN201480052866.5A CN105637042B (zh) 2013-09-30 2014-09-30 离型膜及其制造方法
EP14849767.0A EP3053969A4 (fr) 2013-09-30 2014-09-30 Pellicule anti-adhésive et son procédé de fabrication
US15/025,712 US20160237287A1 (en) 2013-09-30 2014-09-30 Release film and manufacturing method therefor

Applications Claiming Priority (4)

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KR20130116294 2013-09-30
KR10-2013-0116294 2013-09-30
KR10-2014-0130362 2014-09-29
KR1020140130362A KR102204965B1 (ko) 2013-09-30 2014-09-29 이형필름 및 이의 제조방법

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WO2018079596A1 (fr) * 2016-10-25 2018-05-03 三菱ケミカル株式会社 Film de démoulage
CN108473694A (zh) * 2015-12-31 2018-08-31 可隆工业株式会社 离型膜及其制造方法
CN111393697A (zh) * 2020-04-26 2020-07-10 东莞市鼎力薄膜科技有限公司 一种层片式电容用离型膜及其制备方法
CN113801475A (zh) * 2020-05-27 2021-12-17 台科三维科技股份有限公司 低离型力组合物及使用其进行高速三维打印的方法
CN114395154A (zh) * 2022-01-06 2022-04-26 四川东材科技集团股份有限公司 一种pet基材的耐高温离型膜及其制备方法
CN114456428A (zh) * 2022-03-16 2022-05-10 江苏邦宇薄膜技术有限公司 一种mlcc用离型膜的制备方法
CN114605936A (zh) * 2022-01-26 2022-06-10 金丝楠膜(上海)科技有限公司 一种防水卷材及其制备方法和糙化面层的制备方法

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CN108473694A (zh) * 2015-12-31 2018-08-31 可隆工业株式会社 离型膜及其制造方法
JP2019506312A (ja) * 2015-12-31 2019-03-07 コーロン インダストリーズ インク 離型フィルムおよびその製造方法
CN108473694B (zh) * 2015-12-31 2021-04-20 可隆工业株式会社 离型膜及其制造方法
WO2018079596A1 (fr) * 2016-10-25 2018-05-03 三菱ケミカル株式会社 Film de démoulage
CN111393697A (zh) * 2020-04-26 2020-07-10 东莞市鼎力薄膜科技有限公司 一种层片式电容用离型膜及其制备方法
CN111393697B (zh) * 2020-04-26 2022-07-26 东莞市鼎力薄膜科技有限公司 一种层片式电容用离型膜及其制备方法
CN113801475A (zh) * 2020-05-27 2021-12-17 台科三维科技股份有限公司 低离型力组合物及使用其进行高速三维打印的方法
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CN114456428A (zh) * 2022-03-16 2022-05-10 江苏邦宇薄膜技术有限公司 一种mlcc用离型膜的制备方法

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