JP2018154130A5

JP2018154130A5 -

Info

Publication number: JP2018154130A5
Application number: JP2018048632A
Authority: JP
Filing date: 2018-03-15
Publication date: 2020-10-01
Anticipated expiration: 2038-03-15

Description

[６]
厚さが１０〜２００μｍである芳香族ポリイミドフィルムと、環状ジメチルシロキサン４量体〜１５量体の含有量が２５０質量ｐｐｍより多く,補強性充填剤としてヒュームドシリカを含有し、硬化物のＪＩＳＫ６２４９で規定する伸びが３８０％以上であり、１００％伸張時の引張応力が０.２０〜１.３５ＭＰａであるヒドロシリル化反応による加熱硬化型液状シリコーンゴム組成物（Ｉ）または、さらに（Ｂ）有機官能性オルガノアルコキシシランもしくはその部分加水分解縮合物を含有する前記ヒドロシリル化反応よる加熱硬化型液状シリコーンゴム組成物（ＩＩ）とを密接させ、加圧下で９０℃以上１４５℃以下で加熱して該シリコーンゴム組成物を１次硬化させ、次いで、熱気中に、環状ジメチルシロキサン４量体〜１５量体の含有量が２５０質量ｐｐｍ以下になるまで置いて２次硬化させることを特徴とする、ヘッドスペースガスクロマトグラフ分析法用またはヘッドスペースガスクロマトグラフ質量分析法用バイアルの開口部封止用のセプタムを形成するための積層シートであって、厚さが１０〜２００μｍである芳香族ポリイミドフィルムと、厚さが１.２〜５ｍｍであり,環状ジメチルシロキサン４量体〜１５量体の含有量が２５０質量ｐｐｍ以下であり,補強性充填剤として（Ａ）ヒュームドシリカを含有し、ＪＩＳＫ６２４９で規定する伸びが３８０％以上であり、１００％伸張時の引張応力が０.２０〜１.３５ＭＰａであるヒドロシリル化反応硬化シリコーンゴム層（Ｉ）または、さらに（Ｂ）有機官能性オルガノアルコキシシランもしくはその部分加水分解縮合物を含有する前記ヒドロシリル化反応硬化シリコーンゴム層（ＩＩ）とが接着して積層しており、縦１２０ｍｍ,横１２０ｍｍの正方形の積層シート試験片の四隅は、半円弧の一端の形状またはＣ字の一端の形状に湾曲することがなく、四隅の平均反り値が３５ｍｍ以下である積層シートの製造方法。 [6]
The content of the aromatic polyimide film having a thickness of 10 to 200 μm and the cyclic dimethylsiloxane tetramer to 15-mer is more than 250% by mass ppm, and fumed silica is contained as a reinforcing filler. A heat-curable liquid silicone rubber composition (I) by a hydrosilylation reaction in which the elongation specified in K 6249 is 380% or more and the tensile stress at 100% elongation is 0.20 to 1.35 MPa, or (B). ) The heat-curable liquid silicone rubber composition (II) by the hydrosilylation reaction containing organic functional organoalkoxysilane or a partial hydrolysis condensate thereof is brought into close contact with the composition and heated at 90 ° C. or higher and 145 ° C. or lower under pressure. The silicone rubber composition is first-cured, and then placed in hot air until the content of the cyclic dimethylsiloxane tetramer to 15-mer is 250% by mass or less to be secondarily cured. , A laminated sheet for forming a septum for sealing the opening of a vial for headspace gas chromatograph analysis or headspace gas chromatograph mass analysis, and an aromatic polyimide film having a thickness of 10 to 200 μm. The thickness is 1.2 to 5 mm, the content of cyclic dimethylsiloxane tetramer to 15-mer is 250 mass ppm or less, (A) fumed silica is contained as a reinforcing filler, and JIS K The hydrosilylation reaction-curable silicone rubber layer (I) or (B) organic functional organoalkoxy having an elongation of 6249 or more and a tensile stress at 100% elongation of 0.20 to 1.35 MPa. The hydrosilylation reaction-cured silicone rubber layer (II) containing silane or a partially hydrolyzed condensate thereof is adhered and laminated, and the four corners of a square laminated sheet test piece having a length of 120 mm and a width of 120 mm are semi-arc. without having to bend the the shape of one end of the one end of the shape or C-shape, method for producing a laminated sheet average warpage value of the four corners is less than 35 mm.

[７]
厚さが１０〜２００μｍである芳香族ポリイミドフィルムと、厚さが１.２〜５ｍｍであり,環状ジメチルシロキサン４量体〜１５量体の含有量が２５０質量ｐｐｍ以下であり,補強性充填剤として（Ａ）ヒュームドシリカを含有し、ＪＩＳＫ６２４９で規定する伸びが３８０％以上であり,１００％伸張時の引張応力が０.２０〜１.３５ＭＰａであるヒドロシリル化反応硬化シリコーンゴム層（Ｉ）または、さらに（Ｂ）有機官能性オルガノアルコキシシランもしくはその部分加水分解縮合物を含有する前記ヒドロシリル化反応硬化シリコーンゴム層（ＩＩ）とが接着状態で積層しており、ＪＩＳＫ６８５４−２（接着剤−剥離接着強さ試験方法−第２部：１８０度剥離）に基づく剥離接着強さが５Ｎ／２５ｍｍ以上であり、縦１２０ｍｍ,横１２０ｍｍの正方形の積層シート試験片の四隅は,半円弧の一端の形状またはＣ字の一端の形状に湾曲することがなく,四隅の平均反り値が３５ｍｍ以下である積層シートからなることを特徴とする、ヘッドスペースガスクロマトグラフ分析法用またはヘッドスペースガスクロマトグラフ質量分析法用バイアルの開口部封止用セプタム。 [7]
An aromatic polyimide film having a thickness of 10 to 200 μm, a thickness of 1.2 to 5 mm, a cyclic dimethylsiloxane tetramer to a 15-mer content of 250 mass ppm or less, and a reinforcing filler. (A) A hydrosilylation reaction-cured silicone rubber layer containing fumed silica, having an elongation of 380% or more specified by JIS K 6249, and having a tensile stress at 100% elongation of 0.20 to 1.35 MPa. JIS K6854-2 (I) or (B) the hydrosilylation reaction-curable silicone rubber layer (II) containing an organic functional organoalkoxysilane or a partially hydrolyzed condensate thereof is laminated in an adhesive state. Adhesive-Peeling bond strength test method-Part 2: 180 degree peeling) has a peeling bond strength of 5N / 25mm or more, and the four corners of a square laminated sheet test piece with a length of 120mm and a width of 120mm are semi-arc. For headspace gas chromatograph analysis method or headspace gas chromatograph, characterized in that it is composed of a laminated sheet having an average warpage value of 35 mm or less at four corners without being curved into the shape of one end or the shape of one end of a C shape. Septam for sealing the opening of vials for mass analysis.

Claims

An aromatic polyimide film having a thickness of 10 to 200 μm and a thickness of a laminated sheet for producing a septum for sealing an opening of a vial for headspace gas chromatograph analysis or headspace gas chromatograph mass analysis. Is 1.2 to 5 mm, the content of cyclic dimethylsiloxane tetramer to 15-mer is 250 mass ppm or less, and (A) fumed silica is contained as a reinforcing filler, which is specified in JIS K 6249. Hydrosilylation reaction-cured silicone rubber layer (I) having an elongation of 380% or more and a tensile stress at 100% elongation of 0.20 to 1.35 MPa, or (B) an organically functional organoalkoxysilane or its own. The hydrosilylation reaction-cured silicone rubber layer (II) containing a partially hydrolyzed condensate is laminated in an adhesive state, and JIS K6854-2 (adhesive-peeling adhesive strength test method-Part 2: 180 degrees The peeling adhesive strength based on (peeling) is 5N / 25mm or more, and the four corners of a square laminated sheet test piece having a length of 120 mm and a width of 120 mm may be curved into the shape of one end of a semi-arc or the shape of one end of a C-shape. A laminated sheet characterized in that the average warpage value of the four corners is 35 mm or less.

An aromatic polyimide film having a thickness of 10 to 200 μm and a cyclic dimethylsiloxane tetramer to 15-mer having a content of 250 mass ppm or less, and containing (A) fumed silica as a reinforcing filler. A heat-curable liquid silicone rubber composition (I) by a hydrosilylation reaction in which the elongation of the cured product specified by JIS K 6249 is 380% or more and the tensile stress at 100% elongation is 0.20 to 1.35 MPa. Further, (B) the heat-curable liquid silicone rubber composition (II) by the hydrosilylation reaction containing the organically functional organoalkoxysilane or a partially hydrolyzed condensate thereof is brought into close contact with each other at 145 ° C. or lower under pressure. A laminated sheet for forming a septum for sealing the opening of a vial for headspace gas chromatograph analysis or headspace gas chromatograph mass analysis, which is characterized by heating and curing, and has a thickness. A polyimide film having a thickness of 10 to 200 μm, a thickness of 1.2 to 5 mm, a content of cyclic dimethylsiloxane tetramer to 15-mer or less of 250 mass ppm or less, and (A) fume as a reinforcing filler. A hydrosilylation reaction-cured silicone rubber layer (I) containing dosilica, having an elongation of 380% or more as defined by JIS K 6249, and a tensile stress at 100% elongation of 0.20 to 1.35 MPa, or further. (B) The hydrosilylation reaction-curable silicone rubber layer (II) containing an organic functional organoalkoxysilane or a partially hydrolyzed condensate thereof is laminated in an adhesive state, and JIS K6854-2 (adhesive-peeling adhesion ) is laminated. The peeling adhesive strength based on the strength test method-2 part: 180 degree peeling) is 5N / 25mm or more, and the four corners of the square laminated sheet test piece of 120mm in length and 120mm in width have the shape of one end of a semi-arc or A method for manufacturing a laminated sheet in which the shape of one end of a C shape is not curved and the average warpage value of the four corners is 35 mm or less.

An aromatic polyimide film having a thickness of 10 to 200 μm and a hydrosilylation reaction-cured silicone rubber, having a thickness of 1.2 to 5 mm and having a content of cyclic dimethylsiloxane tetramer to 15-mer of 250 mass. It is ppm or less, contains (A) fumed silica as a reinforcing filler, has an elongation of 380% or more specified by JIS K 6249, and has a tensile stress of 0.20 to 1.35 MPa at 100% elongation. The content of the cyclic dimethylsiloxane tetramer to 15-mer is 250 mass ppm or less, and (B) organic functional organoalkoxysilane or a partially hydrolyzed condensate thereof is contained between the silicone rubber sheet and the silicone rubber sheet. Heat-curable liquid silicone rubber composition by hydrosilylation reaction containing (A) fumed silica as a reinforcing filler A heat-curable liquid silicone rubber composition by the liquid hydrosilylation reaction by interposing a thin layer and heating under pressure. The polyimide film and the hydrosilyl for forming a septum for sealing the opening of a vial for headspace gas chromatograph analysis or headspace gas chromatograph mass analysis, which comprises curing a thin layer. The chemical reaction-curing silicone rubber sheet is laminated in an adhesive state, and the four corners of a square laminated sheet test piece with a length of 120 mm and a width of 120 mm may be curved into the shape of one end of a semi-arc or the shape of one end of a C-shape. A method for manufacturing a laminated sheet in which the average warpage value of the four corners is 35 mm or less.

The components (B) are (a) an alkenyl-functional organoalkoxysilane having two or three silicon atom-bonded alkoxy groups in one molecule and (b) two or three silicon atom-bonded alkoxy groups in one molecule. One to three selected from the group consisting of (meth) acrylic functional organoalkoxysilanes and (c) epoxy functional organoalkoxysilanes having two or three silicon atom-bonded alkoxy groups in one molecule. Claimed to be an organically functional organoalkoxysilane, or a co-partially hydrolyzed condensate of the organically functional organoalkoxysilane and (d) an organic titanium compound catalyst, or the organically functional organoalkoxysilanes 2 to 3. Item 3. The method for producing a laminated sheet according to Item 3.

An aromatic polyimide film having a thickness of 10 to 200 μm, a cyclic dimethylsiloxane tetramer to 15-mer having a content of more than 250 mass ppm, containing fumed silica as a reinforcing filler, and (B) organic. Containing functional organoalkoxysilane or a partially hydrolyzed condensate thereof, the elongation of the cured product specified by JIS K 6249 is 250% or more, and the tensile stress at 100% elongation specified by JIS K 6249 is 0.1. The silicone gel composition is first cured by bringing it into close contact with a heat-curable silicone gel composition by a hydrosilylation reaction at ~ 0.49 MPa and heating at 90 ° C. or higher and 240 ° C. or lower under pressure, and then in hot air. For headspace gas chromatograph analysis method or headspace gas chromatograph mass analysis method, which comprises placing the cyclic dimethylsiloxane tetramer to 15-mer to 250 mass ppm or less and performing secondary curing. A laminated sheet for forming a septum for sealing the opening of a vial, which is an aromatic polyimide film having a thickness of 10 to 200 μm and a cyclic dimethylsiloxane 4 having a thickness of 1.2 to 5 mm. The content of the metric to 15-mer is 250% by mass or less, (A) fumed silica is contained as a reinforcing filler, and (B) organic functional organoalkoxysilane or a partially hydrolyzed condensate thereof is contained. However, with a hydrosilylation reaction-cured silicone gel layer in which the elongation of the cured product specified by JIS K 6249 is 250% or more, and the tensile stress at 100% elongation specified by JIS K 6249 is 0.15 to 0.49 MPa. The four corners of the square laminated sheet test piece with a length of 120 mm and a width of 120 mm are not curved into the shape of one end of a semi-arc or the shape of one end of a C-shape, and the average warpage value of the four corners. A method for producing a laminated sheet having a thickness of 35 mm or less.

The content of the aromatic polyimide film having a thickness of 10 to 200 μm and the cyclic dimethylsiloxane tetramer to 15-mer is more than 250% by mass ppm, and fumed silica is contained as a reinforcing filler. A heat-curable liquid silicone rubber composition (I) by a hydrosilylation reaction in which the elongation specified in K 6249 is 380% or more and the tensile stress at 100% elongation is 0.20 to 1.35 MPa, or (B). ) The heat-curable liquid silicone rubber composition (II) by the hydrosilylation reaction containing organic functional organoalkoxysilane or a partial hydrolysis condensate thereof is brought into close contact with the composition and heated at 90 ° C. or higher and 145 ° C. or lower under pressure. The silicone rubber composition is first-cured, and then placed in hot air until the content of the cyclic dimethylsiloxane tetramer to 15-mer is 250% by mass or less to be secondarily cured. , A laminated sheet for forming a septum for sealing the opening of a vial for headspace gas chromatograph analysis or headspace gas chromatograph mass analysis, and an aromatic polyimide film having a thickness of 10 to 200 μm. The thickness is 1.2 to 5 mm, the content of cyclic dimethylsiloxane tetramer to 15-mer is 250 mass ppm or less, (A) fumed silica is contained as a reinforcing filler, and JIS K The hydrosilylation reaction-curable silicone rubber layer (I) or (B) organic functional organoalkoxy having an elongation of 6249 or more and a tensile stress at 100% elongation of 0.20 to 1.35 MPa. The hydrosilylation reaction-cured silicone rubber layer (II) containing silane or a partially hydrolyzed condensate thereof is laminated in an adhesive state, and the four corners of a square laminated sheet test piece having a length of 120 mm and a width of 120 mm are semi-arc. without having to bend the the shape of one end of the one end of the shape or C-shape, method for producing a laminated sheet average warpage value of the four corners is less than 35 mm.

An aromatic polyimide film having a thickness of 10 to 200 μm, a thickness of 1.2 to 5 mm, a cyclic dimethylsiloxane tetramer to a 15-mer content of 250 mass ppm or less, and a reinforcing filler. (A) A hydrosilylation reaction-cured silicone rubber layer containing fumed silica, having an elongation of 380% or more specified by JIS K 6249, and having a tensile stress at 100% elongation of 0.20 to 1.35 MPa. JIS K6854-2 (I) or (B) the hydrosilylation reaction-curable silicone rubber layer (II) containing an organic functional organoalkoxysilane or a partially hydrolyzed condensate thereof is laminated in an adhesive state. Adhesive-Peeling bond strength test method-Part 2: 180 degree peeling) has a peeling bond strength of 5N / 25mm or more, and the four corners of a square laminated sheet test piece with a length of 120mm and a width of 120mm are semi-arc. For headspace gas chromatograph analysis method or headspace gas chromatograph, characterized in that it is composed of a laminated sheet having an average warpage value of 35 mm or less at four corners without being curved into the shape of one end or the shape of one end of a C shape. Septam for sealing the opening of vials for mass analysis.

It is a septum composed of a laminate of an aromatic polyimide film and a hydrosilylation reaction-curing silicone rubber layer, and the hydrosilylation reaction-curing silicone rubber layer contains (A) fumed silica as a reinforcing filler and serves as a cross-linking agent. A cured product of a hydrosilylation reaction-curable silicone rubber composition containing a methylhydrogenpolysiloxane having at least three hydrosilyl groups and a hydrodimethylsiloxy group-blocking dimethylpolysiloxane (polymerization degree 3 or less) at both ends of the molecular chain. The septum is characterized by.

The septum according to claim 8, wherein the hydrosilylation reaction-curable silicone rubber composition further contains (B) an organic functional organoalkoxysilane or a partially hydrolyzed condensate thereof.