WO2013145475A1 - 剥離シート - Google Patents
剥離シート Download PDFInfo
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- WO2013145475A1 WO2013145475A1 PCT/JP2012/083126 JP2012083126W WO2013145475A1 WO 2013145475 A1 WO2013145475 A1 WO 2013145475A1 JP 2012083126 W JP2012083126 W JP 2012083126W WO 2013145475 A1 WO2013145475 A1 WO 2013145475A1
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- polydimethylsiloxane
- release agent
- release sheet
- release
- average molecular
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- 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
- C08J7/0427—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
- C08J7/044—Forming conductive coatings; Forming coatings having anti-static properties
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/56—Organo-metallic compounds, i.e. organic compounds containing a metal-to-carbon bond
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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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
- C09D183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
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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
- 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
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- 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
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- 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
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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
- 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 sheet on which an adhesive layer such as an adhesive sheet is laminated.
- the release sheet for the pressure-sensitive adhesive sheet a sheet composed of a substrate and a release agent layer formed on one side thereof is generally used (for example, Patent Document 1).
- Many release sheets for pressure-sensitive adhesive sheets transport the base material by roll-to-roll, apply the pressure-sensitive adhesive on the base material, and after drying, the pressure-sensitive adhesive layer surface and the release sheet surface of the release sheet are attached. Often used to match.
- the roll conveyance speed is often constant, and the release sheet is rarely exposed to the atmosphere for a long time.
- a back cracking process (cut or half cut) may be performed on the release sheet in a pre-process for pasting the adhesive layer of the adhesive sheet and the release agent layer of the release sheet.
- the release agent layer of the release sheet may be exposed to the atmosphere for a long time.
- the release agent layer of the release sheet is exposed to the atmosphere for a long time, there is a problem that the release force of the release agent layer on the pressure-sensitive adhesive layer becomes larger than the release force before exposure to the atmosphere.
- a heavy peelable sheet having a high peel force tends to have a significant increase in peel force due to atmospheric exposure.
- the present invention has been made in view of such a situation, and a release sheet capable of suppressing an increase in peel force even when the release agent layer of the release sheet is exposed to the atmosphere for a long time.
- the purpose is to provide.
- the present invention provides a release sheet comprising a substrate and a release agent layer formed on at least one surface of the substrate, wherein the release agent layer is at least in one molecule.
- a release agent composition comprising a first polydimethylsiloxane having two alkenyl groups and a second polydimethylsiloxane having at least two hydrosilyl groups in one molecule, wherein the first polydimethylsiloxane In a total of 30 g of dimethylsiloxane and the second polydimethylsiloxane, 0.40 to 5.25 mmol of the alkenyl group, 7.00 to 120.00 mmol of the hydrosilyl group, and the alkenyl group (a ) And a release agent composition having a molar ratio (b / a) of the hydrosilyl group (b) to 3.0 to 70.0.
- invention 1 even if it is a case where the release agent layer of a peeling sheet is exposed to air
- the weight average molecular weight of the first polydimethylsiloxane is preferably 200000 to 1300000, and the weight average molecular weight of the second polydimethylsiloxane is preferably 300 to 1200 (Invention). 2).
- the release agent composition preferably further contains a platinum group metal compound as a catalyst (Invention 3).
- the peel force change rate represented by the formula is 30% or less (Invention 4).
- the release sheet according to the present invention even when the release agent layer of the release sheet is exposed to the atmosphere for a long time, an increase in the release force can be suppressed, and when the release sheet is released from the adhesive sheet It is possible to reduce the peeling failure.
- the release sheet 1 includes a base material 11 and a release agent layer 12 formed on one surface of the base material 11.
- the substrate 11 is not particularly limited, and any one of conventionally known materials can be appropriately selected and used.
- a substrate 11 include films made of polyesters such as polyethylene terephthalate and polyethylene naphthalate, polyolefins such as polypropylene and polymethylpentene, polycarbonates, and plastics such as polyvinyl acetate.
- it may be a multilayer of two or more layers of the same type or different types.
- a polyester film is preferable, a polyethylene terephthalate film is particularly preferable, and a biaxially stretched polyethylene terephthalate film is more preferable.
- a surface treatment by an oxidation method or a concavo-convex method on one side or both sides as desired for the purpose of improving the adhesiveness with the release agent layer 12 provided on the surface, a surface treatment by an oxidation method or a concavo-convex method on one side or both sides as desired, Alternatively, primer treatment can be performed.
- the oxidation method include corona discharge treatment, plasma discharge treatment, chromium oxidation treatment (wet), flame treatment, hot air treatment, ozone, ultraviolet irradiation treatment, and the like.
- Examples include a thermal spraying method.
- These surface treatment methods are appropriately selected according to the type of the base film, but generally, a corona discharge treatment method is preferably used from the viewpoints of effects and operability.
- the base material 11 is paper such as glassine paper, clay coated paper, resin coated paper, laminated paper (polyethylene laminated paper, polypropylene laminated paper, etc.), nonwoven fabric, or metal foil. Etc. can also be used.
- the thickness of the substrate 11 is usually 10 to 300 ⁇ m, preferably 15 to 200 ⁇ m, and particularly preferably 20 to 125 ⁇ m.
- the release agent layer 12 in the present embodiment is formed using the following release agent composition.
- the release agent composition in the present embodiment is, as an addition reaction type silicone resin, a first polydimethylsiloxane having at least two alkenyl groups in one molecule and a second polysilylsiloxane having at least two hydrosilyl groups in one molecule. 2 polydimethylsiloxane.
- alkenyl group contained in the first polydimethylsiloxane examples include monovalent hydrocarbon groups such as vinyl group, allyl group, propenyl group, butenyl group, pentenyl group, hexenyl group, heptenyl group, and octenyl group.
- the group is particularly preferred.
- the alkenyl group is contained in an amount of 0.40 to 5.25 mmol, preferably 0.50 to 5.20 mmol, in a total of 30 g of the first polydimethylsiloxane and the second polydimethylsiloxane.
- the hydrosilyl group is contained in 7.00 to 120.00 mmol, preferably 8.00 to 115.00 mmol, in a total of 30 g of the first polydimethylsiloxane and the second polydimethylsiloxane.
- the molar ratio (b / a) of the hydrosilyl group (b) to the alkenyl group (a) is 3.0 to 70.0, preferably 3.5 to 65.0.
- the release agent layer 12 is formed using a release agent composition that satisfies the above conditions, the release agent layer 12 has a release force even when the release agent layer 12 is exposed to the atmosphere for a long time. Increase is suppressed. The reason for this is not necessarily clear, but the release agent layer 12 formed using the release agent composition satisfying the above conditions has low polarity, and dust or dust with high polarity is difficult to adhere to the release agent layer 12. This is probably because of this.
- the amount of alkenyl groups in a total of 30 g of the first polydimethylsiloxane and the second polydimethylsiloxane is less than 0.40 mmol, or the amount of hydrosilyl groups is less than 7.00 mmol, Insufficient curing occurs, and silicone transfer to the pressure-sensitive adhesive layer or the like of the coating machine or the pressure-sensitive adhesive sheet becomes a problem, and the peelability is adversely affected.
- the first polydimethylsiloxane preferably does not have a hydrosilyl group
- the second polydimethylsiloxane preferably does not have an alkenyl group
- the weight average molecular weight of the first polydimethylsiloxane is preferably 20000 to 1300000, particularly preferably 300000 to 1200000.
- the weight average molecular weight of the second polydimethylsiloxane is preferably 300 to 1400, particularly preferably 500 to 1200.
- the weight average molecular weight in this specification is the value of polystyrene conversion measured by the gel permeation chromatography (GPC) method.
- the release agent composition preferably contains a catalyst.
- the catalyst is not particularly limited as long as it can cure the release agent composition according to the present embodiment, and among them, a platinum group metal compound is preferable.
- the platinum group metal compounds include fine platinum, fine platinum adsorbed on a carbon powder carrier, chloroplatinic acid, alcohol-modified chloroplatinic acid, olefin complexes of chloroplatinic acid, palladium, rhodium and the like. .
- the release agent composition contains such a catalyst, the curing reaction of the release agent composition can proceed more efficiently.
- the content of the catalyst in the release agent composition is preferably about 1 to 1000 ppm with respect to the total amount of components other than the catalyst.
- the release agent composition may contain a reaction inhibitor, an adhesion improver, etc. in addition to the first and second polydimethylsiloxanes and the catalyst.
- the thickness (basis weight) of the release agent layer 12 is not particularly limited, but is preferably 0.01 to 3 g / m 2 , and particularly preferably 0.05 to 2 g / m 2 .
- the thickness of the release agent layer 12 is less than 0.01 g / m 2 , the function as the release agent layer 12 may not be sufficiently exhibited depending on the material constituting the release agent layer 12 or the like.
- the thickness of the release agent layer 12 exceeds 3 g / m 2 , blocking may occur when the release sheet 1 is wound into a roll, resulting in a failure in feeding.
- the release agent layer 12 can be formed by applying a release agent composition and, optionally, a coating solution containing a diluent to one surface of the substrate 11, and then drying and curing.
- a coating method for example, gravure coating method, bar coating method, spray coating method, spin coating method, knife coating method, roll coating method, die coating method and the like can be used.
- the diluent is not particularly limited, and various types can be used.
- hydrocarbon compounds such as toluene, hexane, heptane, acetone, ethyl acetate, methyl ethyl ketone, methyl isobutyl ketone, and mixtures thereof are used.
- the release agent composition coated as described above is preferably thermoset.
- the heating temperature is preferably 80 to 180 ° C.
- the heating time is preferably about 10 to 90 seconds.
- the rate of change in peel force represented by the formula is preferably 30% or less, particularly preferably 25% or less, further preferably 15% or less, and most preferably 10% or less. Further, since the peel force does not decrease excessively, the peel force change rate is preferably ⁇ 30% or more.
- the release sheet 1 In the clean room, the release sheet 1 is exposed by being suspended perpendicular to the ground. In the case of exposure that does not hang vertically with respect to the ground, even in a clean room, there is a small amount of dust and dirt, so if dust or dirt accumulates on the surface of the release agent layer 12, the influence of dust or dust on the peel force measurement Accordingly, the peeling force may not be stable and an accurate value may not be obtained.
- another layer such as an antistatic layer may be provided between the surface of the substrate 1 opposite to the release agent layer 12 and between the substrate 1 and the release agent layer 12.
- Example 1 As the first polydimethylsiloxane, a vinyl-modified silicone resin (weight average molecular weight: 330000) having at least two vinyl groups in the polydimethylsiloxane structure, and as the second polydimethylsiloxane, in the polydimethylsiloxane structure.
- This is a mixture of polymethylhydrogensiloxane having at least two hydrosilyl groups (weight average molecular weight: 1000) and non-functional silicone resin having no functional group in the structure of the silicone resin (weight average molecular weight: 490000).
- a silicone resin solution was prepared by diluting an addition reaction type organopolysiloxane having a weight average molecular weight of 350,000 (release agent composition A) with toluene so as to have a solid content of 30% by mass.
- release agent composition A release agent composition A
- To 100 parts by mass of this silicone resin solution 2 parts by mass of a platinum-based catalyst (manufactured by Dow Corning Toray, BY24-835) is added, and the solid content concentration is adjusted to 1.5% by mass with toluene.
- the obtained coating liquid is placed on a polyethylene terephthalate film (Mitsubishi Resin, T-100, thickness 38 ⁇ m) as a base material so that the film thickness after drying becomes 0.09 g / m 2. After applying uniformly by the bar coat method, it is dried at 130 ° C. for 1 minute, and the release agent layer is covered with the substrate so that the release agent layer is not exposed, and the release agent layer is laminated on the substrate. A sheet was obtained.
- a polyethylene terephthalate film Mitsubishi Resin, T-100, thickness 38 ⁇ m
- Example 2 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 330000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 310,000, which is a mixture with a polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the polydimethylsiloxane structure.
- a release sheet was produced in the same manner as in Example 1 except that (release agent composition B) was used.
- Example 3 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 330000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 330000, which is a mixture with a polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the polydimethylsiloxane structure.
- a release sheet was produced in the same manner as in Example 1 except that the (release agent composition C) was used.
- Example 4 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 1200000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 118,000, which is a mixture with a polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the polydimethylsiloxane structure.
- a release sheet was produced in the same manner as in Example 1 except that (release agent composition D) was used.
- Example 5 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 1000000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, an addition reaction having a weight average molecular weight of 537,000.
- a release sheet was prepared in the same manner as in Example 1 except that type organopolysiloxane (release agent composition E) was used.
- Example 6 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 1000000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, and an addition reaction having a weight average molecular weight of 613,000.
- a release sheet was produced in the same manner as in Example 1 except that type organopolysiloxane (release agent composition F) was used.
- Example 7 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 290000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, and an addition reaction having a weight average molecular weight of 285,000.
- a release sheet was prepared in the same manner as in Example 1 except that type organopolysiloxane (release agent composition G) was used.
- Example 8 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 1000000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, an addition reaction having a weight average molecular weight of 650000.
- a release sheet was prepared in the same manner as in Example 1 except that type organopolysiloxane (release agent composition H) was used.
- Example 1 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 330000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 167,000, which is a mixture with a polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the polydimethylsiloxane structure.
- a release sheet was produced in the same manner as in Example 1 except that the (release agent composition I) was used.
- Example 2 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 330000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 200,000, which is a mixture with polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane
- a release sheet was produced in the same manner as in Example 1 except that the (release agent composition J) was used.
- Example 3 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 330000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 249000, which is a mixture with polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane.
- a release sheet was produced in the same manner as in Example 1 except that (release agent composition K) was used.
- Example 4 instead of the release agent composition A in Example 1, a vinyl-modified silicone resin (weight average molecular weight: 300,000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane,
- the polydimethylsiloxane is an addition reaction type organopolysiloxane having a weight average molecular weight of 300,000, which is a mixture with a polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the polydimethylsiloxane structure.
- a release sheet was produced in the same manner as in Example 1 except that (release agent composition L) was used.
- a vinyl-modified silicone resin (weight average molecular weight: 290000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, and an addition reaction having a weight average molecular weight of 295,000.
- a release sheet was prepared in the same manner as in Example 1 except that type organopolysiloxane (release agent composition M) was used.
- a vinyl-modified silicone resin (weight average molecular weight: 1000000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, and an addition reaction having a weight average molecular weight of 671000.
- a release sheet was prepared in the same manner as in Example 1 except that type organopolysiloxane (release agent composition N) was used.
- a vinyl-modified silicone resin (weight average molecular weight: 1000000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the structure of polydimethylsiloxane and a silica filler, and an addition reaction having a weight average molecular weight of 692,000.
- a release sheet was produced in the same manner as in Example 1 except that type organopolysiloxane (release agent composition O) was used.
- a vinyl-modified silicone resin (weight average molecular weight: 1000000) having at least two vinyl groups in the structure of polydimethylsiloxane as the first polydimethylsiloxane
- the polydimethylsiloxane is a mixture of polymethylhydrogensiloxane (weight average molecular weight: 1000) having at least two hydrosilyl groups in the polydimethylsiloxane structure and a silica filler, and an addition reaction having a weight average molecular weight of 715,000.
- a release sheet was prepared in the same manner as in Example 1 except that type organopolysiloxane (release agent composition P) was used.
- deuterated chloroform manufactured by Kanto Chemical Co., Inc., purity 99.8%
- pyrazine Tokyo Chemical Industry Co., Ltd., PO554
- NMR measurement was performed using the nuclear magnetic resonance apparatus (the BRUKER company make, NMR * Fourier300), and each functional group amount (mmol) of the vinyl group and the hydrosilyl group was quantified.
- Polyester adhesive tape manufactured by Nitto Denko Corporation, product number: No. 31B, 20 mm
- the width was applied by reciprocating a 2 kg roller once to obtain a test piece for measuring peel force.
- the peel strength of the obtained test piece was measured.
- a tensile tester product name: AG-IS 500N (load cell 20N) manufactured by Shimadzu Corporation was used for measuring the peeling force. Specifically, the peeling sheet side of the test piece is fixed to a SUS plate, and the polyester adhesive tape is peeled at a speed of 0.3 m / min while being distorted at 180 °. The peeling force (mN / 20 mm at this time) ) was measured. Further, the peel force change rate (%) was calculated from the obtained peel force according to the following formula. The results are shown in Table 2, respectively.
- Peeling force change rate (%) ⁇ (peeling force Y ⁇ peeling force X) / peeling force X ⁇ ⁇ 100 Peeling force X: Peeling force when there is no exposure Peeling force Y: Peeling force when exposed for 1 or 7 days
- the release sheet of the present invention is suitably used for a release sheet that is subjected to back cracking and the like, and the release agent layer is exposed to the atmosphere for a long time.
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Abstract
Description
{(剥離力Y-剥離力X)/剥離力X}×100%
の式で表わされる剥離力変化率が、30%以下であることが好ましい(発明4)。
図1に示すように、本実施形態に係る剥離シート1は、基材11と、基材11の一方の面に形成された剥離剤層12とを備えて構成される。
大気曝露なしの状態における剥離シート1に対する日東電工社製ポリエステル粘着テープNo.31Bの180°剥離力(mN/20mm)を剥離力X、
クラス1万(ISOクラス7)、温度23℃および湿度50%RHの条件のクリーンルームにて7日間大気曝露した剥離シート1に対する日東電工社製ポリエステル粘着テープNo.31Bの180°剥離力(mN/20mm)を剥離力Yとしたときに、
{(剥離力Y-剥離力X)/剥離力X}×100%
の式で表わされる剥離力変化率が、30%以下であることが好ましく、25%以下であることが特に好ましく、15%以下であることがさらに好ましく、10%以下であることが最も好ましい。また、剥離力が減少し過ぎないために、剥離力変化率は、-30%以上であることが好ましい。
第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:330000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリコーンレジンの構造中に官能基を有さない無官能性シリコーンレジン(重量平均分子量:490000)との混合物である、重量平均分子量が350000の付加反応型オルガノポリシロキサン(剥離剤組成物A)を、固形分30質量%となるようにトルエンで希釈して、シリコーン樹脂溶液を調製した。このシリコーン樹脂溶液100質量部に白金系触媒(東レ・ダウコーニング社製,BY24-835)2質量部を加え、トルエンで固形分濃度が1.5質量%となるように調整し、塗工液を得た。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:330000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が310000の付加反応型オルガノポリシロキサン(剥離剤組成物B)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:330000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が330000の付加反応型オルガノポリシロキサン(剥離剤組成物C)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1200000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が1180000の付加反応型オルガノポリシロキサン(剥離剤組成物D)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1000000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が537000の付加反応型オルガノポリシロキサン(剥離剤組成物E)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1000000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が613000の付加反応型オルガノポリシロキサン(剥離剤組成物F)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:290000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が285000の付加反応型オルガノポリシロキサン(剥離剤組成物G)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1000000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が650000の付加反応型オルガノポリシロキサン(剥離剤組成物H)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:330000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が167000の付加反応型オルガノポリシロキサン(剥離剤組成物I)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:330000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が200000の付加反応型オルガノポリシロキサン(剥離剤組成物J)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:330000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が249000の付加反応型オルガノポリシロキサン(剥離剤組成物K)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:300000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)との混合物である、重量平均分子量が300000の付加反応型オルガノポリシロキサン(剥離剤組成物L)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:290000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が295000の付加反応型オルガノポリシロキサン(剥離剤組成物M)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1000000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が671000の付加反応型オルガノポリシロキサン(剥離剤組成物N)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1000000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が692000の付加反応型オルガノポリシロキサン(剥離剤組成物O)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例1における剥離剤組成物Aの替わりに、第1のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にビニル基を少なくとも2個有するビニル変性シリコーン樹脂(重量平均分子量:1000000)と、第2のポリジメチルシロキサンとして、ポリジメチルシロキサンの構造中にヒドロシリル基を少なくとも2個有するポリメチルハイドロジェンシロキサン(重量平均分子量:1000)と、シリカフィラーとの混合物である、重量平均分子量が715000の付加反応型オルガノポリシロキサン(剥離剤組成物P)を使用する以外、実施例1と同様にして剥離シートを作製した。
実施例および比較例で使用した剥離剤組成物A~Pにおける各官能基(ビニル基・ヒドロシリル基)の量を、次の測定方法に従って測定した。
クラス1万(ISOクラス7)、温度23℃および湿度50%RHの条件のクリーンルームにて、実施例および比較例で得られた剥離シートを地面に対し垂直に吊るし、1日または7日間大気曝露した。
剥離力変化率(%)={(剥離力Y-剥離力X)/剥離力X}×100
剥離力X:曝露なしのときの剥離力
剥離力Y:曝露1日又は7日のときの剥離力
11…基材
12…剥離剤層
Claims (4)
- 基材と、少なくとも前記基材の一方の面に形成された剥離剤層とを備えた剥離シートにおいて、
前記剥離剤層は、1分子中に少なくとも2個のアルケニル基を有する第1のポリジメチルシロキサンと、1分子中に少なくとも2個のヒドロシリル基を有する第2のポリジメチルシロキサンとを含有する剥離剤組成物であって、前記第1のポリジメチルシロキサンおよび前記第2のポリジメチルシロキサンの合計30g中に、前記アルケニル基を0.40~5.25mmol含有し、前記ヒドロシリル基を7.00~120.00mmol含有し、かつ前記アルケニル基(a)に対する前記ヒドロシリル基(b)のモル比(b/a)が3.0~70.0である剥離剤組成物を使用して形成されてなる
ことを特徴とする剥離シート。 - 前記第1のポリジメチルシロキサンの重量平均分子量は、200000~1300000であり、前記第2のポリジメチルシロキサンの重量平均分子量は、300~1200であることを特徴とする請求項1に記載の剥離シート。
- 前記剥離剤組成物は、触媒として白金族金属系化合物をさらに含有することを特徴とする請求項1または2に記載の剥離シート。
- 大気曝露なしの状態における前記剥離シートに対する日東電工社製ポリエステル粘着テープNo.31Bの180°剥離力(mN/20mm)を剥離力X、クラス1万(ISOクラス7)、温度23℃および湿度50%RHの条件のクリーンルームにて7日間大気曝露した前記剥離シートに対する日東電工社製ポリエステル粘着テープNo.31Bの180°剥離力(mN/20mm)を剥離力Yとしたときに、
{(剥離力Y-剥離力X)/剥離力X}×100%
の式で表わされる剥離力変化率が、30%以下であることを特徴とする請求項1~3のいずれか一項に記載の剥離シート。
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JP2005314510A (ja) * | 2004-04-28 | 2005-11-10 | Shin Etsu Chem Co Ltd | 硬化性シリコ−ン剥離剤組成物 |
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JPS63218763A (ja) * | 1987-03-06 | 1988-09-12 | Shin Etsu Chem Co Ltd | 硬化性オルガノポリシロキサン組成物 |
JP2003055552A (ja) * | 2001-08-16 | 2003-02-26 | Shin Etsu Chem Co Ltd | 剥離紙用シリコーン組成物及び剥離紙 |
JP2005314510A (ja) * | 2004-04-28 | 2005-11-10 | Shin Etsu Chem Co Ltd | 硬化性シリコ−ン剥離剤組成物 |
JP2008214497A (ja) * | 2007-03-05 | 2008-09-18 | Shin Etsu Chem Co Ltd | フィルム用無溶剤型シリコーン剥離剤組成物及びそれを用いてなる剥離フィルム |
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JP2013202830A (ja) | 2013-10-07 |
US9279065B2 (en) | 2016-03-08 |
CN104203569A (zh) | 2014-12-10 |
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