JP2011074191A - Adhesive composition and adhesive sheet using the same - Google Patents
Adhesive composition and adhesive sheet using the same Download PDFInfo
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- JP2011074191A JP2011074191A JP2009226480A JP2009226480A JP2011074191A JP 2011074191 A JP2011074191 A JP 2011074191A JP 2009226480 A JP2009226480 A JP 2009226480A JP 2009226480 A JP2009226480 A JP 2009226480A JP 2011074191 A JP2011074191 A JP 2011074191A
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 41
- 239000000853 adhesive Substances 0.000 title claims abstract description 39
- 239000000203 mixture Substances 0.000 title claims abstract description 20
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 54
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 54
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004743 Polypropylene Substances 0.000 claims abstract description 9
- 239000004793 Polystyrene Substances 0.000 claims abstract description 9
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 9
- 239000004417 polycarbonate Substances 0.000 claims abstract description 9
- -1 polypropylene Polymers 0.000 claims abstract description 9
- 229920001155 polypropylene Polymers 0.000 claims abstract description 9
- 229920002223 polystyrene Polymers 0.000 claims abstract description 9
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 66
- 239000013032 Hydrocarbon resin Substances 0.000 claims description 12
- 125000002723 alicyclic group Chemical group 0.000 claims description 12
- 229920006270 hydrocarbon resin Polymers 0.000 claims description 12
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 12
- 229920005549 butyl rubber Polymers 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 abstract description 24
- 238000004458 analytical method Methods 0.000 abstract description 18
- 238000007689 inspection Methods 0.000 abstract description 9
- 238000007789 sealing Methods 0.000 abstract description 7
- 238000004811 liquid chromatography Methods 0.000 abstract description 2
- 230000001747 exhibiting effect Effects 0.000 abstract 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 239000010410 layer Substances 0.000 description 18
- 229920006267 polyester film Polymers 0.000 description 15
- 239000003566 sealing material Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 238000003851 corona treatment Methods 0.000 description 5
- 238000004128 high performance liquid chromatography Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 229920001296 polysiloxane Polymers 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 229920005555 halobutyl Polymers 0.000 description 2
- 238000007373 indentation Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 239000013464 silicone adhesive Substances 0.000 description 2
- 239000003522 acrylic cement Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
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- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
本発明は、分析、検査用のマイクロプレートのシールに好適な粘着剤組成物およびそれを用いた粘着シートに関する。 The present invention relates to an adhesive composition suitable for sealing a microplate for analysis and inspection, and an adhesive sheet using the same.
係るマイクロプレートは、例えば以下の特許文献１や非特許文献１、２などに示すように多くのくぼみのついたプラスチック製の箱型の成形品で、分析、検査時の試料保管用に使用される。
Such a microplate is a plastic box-shaped molded product with many indentations as shown in, for example, Patent Document 1 and
くぼみの数が９６穴以上で、１つの穴の容量が数ｍｌのマイクロプレートは、主に高速液体クロマトグラフィーの自動分析用の試料保管用に用いられ、マイクロプレート中の試料は、オートサンプラーによって液体クロマトグラフィーへ搬送される。分析、検査試料は、その試料毎に様々な溶媒に希釈され、マイクロプレートの穴へ入れられ保管されるが、分析、検査までの間、外部物質による汚染防止のためにシール材により穴を塞いで保管する。 A microplate with 96 or more indentations and a volume of one ml of several ml is mainly used for sample storage for automatic analysis of high performance liquid chromatography, and the sample in the microplate is obtained by an autosampler. Delivered to liquid chromatography. Samples for analysis and inspection are diluted with various solvents for each sample and stored in the holes of the microplate. Until the analysis and inspection, the holes are closed with a sealing material to prevent contamination by external substances. Keep in.
高速液体クロマトグラフィーの場合、マイクロプレートからのサンプリングはシリンジ針によるものが多く、この場合のシール材料には、シリンジ針により容易に穴が開くよう厚さ数十μｍのポリエステルフィルムやオレフィン系のフィルム、又はこれらプラスチックフィルムとアルミ箔との複合体が使用される。 In the case of high-performance liquid chromatography, sampling from a microplate is often performed with a syringe needle. In this case, the sealing material is a polyester film or olefin film with a thickness of several tens of micrometers so that holes can be easily opened with the syringe needle. Alternatively, a composite of these plastic film and aluminum foil is used.
シール材となるフィルムとマイクロプレートの接着には、加熱溶融タイプの接着剤を用いる方法と、感圧により接着する粘着剤を用いる方法があり、これらの接着剤は予めシール材のフィルムに塗布され、一体となっている。特に感圧性の粘着タイプのものは、マイクロプレートへのシールの固定に加熱設備を必要とせず、加熱するによる試料の変性も起こらないことから、シール材として適用範囲の広いものとなっている。 There are two methods for bonding the film as the sealing material and the microplate: a method using a heat-melt type adhesive and a method using a pressure-sensitive adhesive, and these adhesives are applied to the sealing material film in advance. , It is one. In particular, the pressure-sensitive adhesive type does not require a heating facility for fixing the seal to the microplate, and the sample is not denatured by heating, so that it has a wide range of application as a sealing material.
マイクロプレートシール用として販売される感圧タイプの粘着シートは、前述のシール材料を支持体として、シリコーン系の粘着剤やアクリル系の粘着剤が塗工されているものが一般的である。 A pressure-sensitive adhesive sheet sold for microplate sealing is generally coated with a silicone-based adhesive or an acrylic-based adhesive using the above-mentioned sealing material as a support.
また、試料を溶解、希釈するための溶媒は各種あるが、一般的にはアセトニトリル、ジメチルスルフォキシド、メタノールが使用される。 There are various solvents for dissolving and diluting the sample, but acetonitrile, dimethyl sulfoxide, and methanol are generally used.
シリコーン系粘着剤の上記の各溶媒に対する溶解度は、アセトニトリルで ５．５％、ジメチルスルフォキシドで１０％となり、また、メタノールに対する溶解度は２６．５％と高い数値となる。 The solubility of the silicone-based adhesive in each of the above solvents is 5.5% for acetonitrile and 10% for dimethyl sulfoxide, and the solubility in methanol is 26.5%.
また、アクリル系の粘着剤は、メタノールに対する溶解度は３％と低いが、アセトニトリルやジメチルスルフォキシドに対する溶解度は９５％以上と高く、溶解してしまう。 An acrylic adhesive has a low solubility in methanol of 3%, but has a high solubility in acetonitrile or dimethyl sulfoxide of 95% or more and dissolves.
従って、シール後のマイクロプレートの搬送等により溶媒と粘着剤が触れた時や、分析時、粘着層を貫通したシリンジ針に粘着剤の付着が起こった場合、溶媒中に粘着剤成分が溶け出し、分析精度を落とすこととなる。このため、溶媒によってシール材を使い分けたり、測定数の数増しをするなど、煩雑な作業を余儀なくされている。 Therefore, when the solvent and adhesive come into contact with the microplate after sealing, etc., or when the adhesive adheres to the syringe needle that penetrates the adhesive layer during analysis, the adhesive component dissolves into the solvent. Analysis accuracy will be reduced. For this reason, complicated work such as using different sealing materials depending on the solvent or increasing the number of measurements is unavoidable.
また、粘着シートの二次加工によりシリンジ注入部の粘着剤を取り除いたタイプのシール材も販売されているが、これは加工工程が追加されるために高価になるという問題もある。 In addition, a type of sealing material in which the pressure-sensitive adhesive in the syringe injection part is removed by secondary processing of the pressure-sensitive adhesive sheet is also sold, but this also has a problem that it is expensive due to an additional processing step.
以上述べたように、従来のマイクロプレートのシールに使用されているシリコーン系およびアクリル系粘着剤は、高速液体クロマトグラフィーによる検査、分析に一般的に使用される一部の溶媒に溶解するため、その溶媒と粘着剤が触れた時や、分析時、粘着層を貫通したシリンジ針に粘着剤の付着が起こった場合、溶媒中に粘着剤成分が溶け出し、分析精度を落とすこととなる。そのため、従来では溶媒によってシール材を使い分けたり、測定数の数増しをするなど、煩雑な作業を余儀なくされていた。あるいは、シリンジ注入部の粘着剤を取り除いたタイプのシール材を使用しなくてはならず、高価なシール材を使用しなければならなかった。 As described above, the silicone-based and acrylic pressure-sensitive adhesives used for sealing conventional microplates are soluble in some solvents commonly used for inspection and analysis by high-performance liquid chromatography. When the solvent and the pressure sensitive adhesive come into contact with each other, or when the pressure sensitive adhesive adheres to the syringe needle penetrating the pressure sensitive adhesive layer during analysis, the pressure sensitive adhesive component dissolves in the solvent, resulting in a decrease in analysis accuracy. For this reason, conventionally, complicated work such as using different sealing materials depending on the solvent or increasing the number of measurements has been unavoidable. Alternatively, a type of sealing material from which the adhesive at the syringe injection portion has been removed must be used, and an expensive sealing material has to be used.
本発明は、上記従来技術の有していた課題を解決するためになされたもので、高速液体クロマトグラフィーによる検査、分析に一般的に使用される溶媒、アセトニトリル、ジメチルスルフォキシド、メタノールに溶解せず、かつ粘着特性に優れ、粘着層を除去する等の作業を必要としない、マイクロプレートのシールに好適な粘着剤組成物およびそれを用いた粘着シートを提供することを目的とする。 The present invention has been made to solve the above-mentioned problems of the prior art, and is dissolved in solvents, acetonitrile, dimethyl sulfoxide, and methanol generally used for inspection and analysis by high performance liquid chromatography. It is an object of the present invention to provide a pressure-sensitive adhesive composition suitable for microplate sealing and a pressure-sensitive adhesive sheet using the pressure-sensitive adhesive composition that is excellent in pressure-sensitive adhesive properties and does not require an operation such as removal of the pressure-sensitive adhesive layer.
本発明の目的を達成するために、本発明の特許請求の範囲に記載のような構成とするものである。 In order to achieve the object of the present invention, the present invention is configured as described in the claims of the present invention.
すなわち、本発明の粘着剤組成物は、アセトニトリル、ジメチルスルフォキシド、メタノールに対する溶解度を３％以下、かつ、ポリプロピレン、ポリスチレン、ポリカーボネートに対する粘着力を０℃〜４０℃の範囲で３Ｎ／１０ｍｍ以上とする。 That is, the pressure-sensitive adhesive composition of the present invention has a solubility in acetonitrile, dimethyl sulfoxide and methanol of 3% or less, and an adhesive strength to polypropylene, polystyrene and polycarbonate of 3 N / 10 mm or more in the range of 0 ° C. to 40 ° C. To do.
この場合、本発明の粘着剤組成物は、ブチルゴム１００重量部に対して、軟化点８５〜１４０℃の脂環族飽和炭化水素樹脂を５〜３０重量部配合する。 In this case, the pressure-sensitive adhesive composition of the present invention contains 5 to 30 parts by weight of an alicyclic saturated hydrocarbon resin having a softening point of 85 to 140 ° C. with respect to 100 parts by weight of butyl rubber.
また、本発明の粘着シートは、アセトニトリル、ジメチルスルフォキシド、メタノールに対する溶解度を３％以下、かつ、ポリプロピレン、ポリスチレン、ポリカーボネートに対する粘着力を０℃〜４０℃の範囲で３Ｎ／１０ｍｍ以上とする。 The pressure-sensitive adhesive sheet of the present invention has a solubility in acetonitrile, dimethyl sulfoxide and methanol of 3% or less, and a pressure-sensitive adhesive force to polypropylene, polystyrene and polycarbonate in the range of 0 ° C. to 40 ° C. to 3 N / 10 mm or more.
この場合、本発明の粘着シートは、上記粘着剤組成物を基材上に塗工する。 In this case, the pressure-sensitive adhesive sheet of the present invention coats the pressure-sensitive adhesive composition on a substrate.
本発明の粘着剤組成物は、アセトニトリル、ジメチルスルフォキシド、メタノールに対する溶解度を３％以下、かつ、ポリプロピレン、ポリスチレン、ポリカーボネートに対する粘着力を０℃〜４０℃の範囲で３Ｎ／１０ｍｍ以上であるから、これをポリエステルフィルム等の基材に塗工した粘着シートは、粘着剤と溶媒の接触があったり、試料のサンプリング時に粘着剤層を通過するシリンジに粘着剤が付着し溶媒中に浸入したとしても、粘着剤が溶媒に溶け出すことがないため、より精度の高い分析を行うことができ、かつマイクロプレートのシールの固定に十分な粘着力を有するため、分析試料への外部物質による汚染を防止することができる。
また、本発明の粘着シートは、アセトニトリル、ジメチルスルフォキシド、メタノールに対する溶解度を３％以下、かつ、ポリプロピレン、ポリスチレン、ポリカーボネートに対する粘着力を０℃〜４０℃の範囲で３Ｎ／１０ｍｍ以上であるから、これをポリエステルフィルム等の基材に塗工した粘着シートは、粘着剤と溶媒の接触があったり、試料のサンプリング時に粘着剤層を通過するシリンジに粘着剤が付着し溶媒中に浸入したとしても、粘着剤が溶媒に溶け出すことがないため、より精度の高い分析を行うことができ、かつマイクロプレートのシールの固定に十分な粘着力を有するため、分析試料への外部物質による汚染を防止することができる。
The pressure-sensitive adhesive composition of the present invention has a solubility in acetonitrile, dimethyl sulfoxide and methanol of 3% or less, and a pressure-sensitive adhesive force to polypropylene, polystyrene and polycarbonate of 3N / 10 mm or more in the range of 0 ° C to 40 ° C. The pressure-sensitive adhesive sheet coated on a substrate such as a polyester film has contact between the pressure-sensitive adhesive and the solvent, or the pressure-sensitive adhesive adheres to the syringe that passes through the pressure-sensitive adhesive layer when the sample is sampled and enters the solvent. However, since the adhesive does not dissolve in the solvent, more accurate analysis can be performed, and because it has sufficient adhesive strength to fix the microplate seal, contamination of the analysis sample by external substances is prevented. Can be prevented.
Further, the pressure-sensitive adhesive sheet of the present invention has a solubility in acetonitrile, dimethyl sulfoxide and methanol of 3% or less, and a pressure-sensitive adhesive force to polypropylene, polystyrene and polycarbonate of 3 N / 10 mm or more in the range of 0 ° C. to 40 ° C. The pressure-sensitive adhesive sheet coated on a substrate such as a polyester film has contact between the pressure-sensitive adhesive and the solvent, or the pressure-sensitive adhesive adheres to the syringe that passes through the pressure-sensitive adhesive layer when the sample is sampled and enters the solvent. However, since the adhesive does not dissolve in the solvent, more accurate analysis can be performed, and because it has sufficient adhesive strength to fix the microplate seal, contamination of the analysis sample by external substances is prevented. Can be prevented.
本発明者は鋭意検討を重ねた結果、エラストマーとしてブチルゴム、粘着付与剤として脂環飽和族炭化水素樹脂を配合することにより、高速液体クロマトグラフィーによる検査、分析に一般的に使用される溶媒、アセトニトリル、ジメチルスルフォキシド、メタノールに溶解せず、かつ、粘着特性に優れたマイクロプレートのシールに好適な粘着剤組成物を見出し、それを用いた粘着シートを開発することができた。 As a result of intensive studies, the inventor blended butyl rubber as an elastomer and an alicyclic saturated hydrocarbon resin as a tackifier, so that a solvent generally used for inspection and analysis by high performance liquid chromatography, acetonitrile The present inventors have found a pressure-sensitive adhesive composition suitable for sealing microplates that does not dissolve in dimethyl sulfoxide and methanol and has excellent adhesive properties, and has been able to develop a pressure-sensitive adhesive sheet using the same.
図１は本発明に係る粘着シート１の実施の一形態を示す拡大断面図である。 FIG. 1 is an enlarged cross-sectional view showing an embodiment of an adhesive sheet 1 according to the present invention.
図示するようにこの粘着シート１は、ポリエステルフィルムなどからなる基材２上に、粘着剤組成物からなる粘着剤層３を備えた構造となっている。
As shown in the figure, this pressure-sensitive adhesive sheet 1 has a structure in which a pressure-sensitive
この粘着剤層３を構成する粘着剤組成物は、具体的には、ブチルゴム１００重量部に対して、軟化点８５℃〜１４０℃の脂環族飽和炭化水素樹脂を５〜３０重量部配合したもので、これをトルエンに溶解し、基材２のポリエステルフィルム上に塗布、乾燥することにより粘着剤層３を作製することができる。
Specifically, the pressure-sensitive adhesive composition constituting the pressure-sensitive
上記ブチルゴムには、レギュラーゴムのほかハロゲン化ブチルゴムを使用できる。これらはムーニー粘度によるレギュラーゴムのグレードやハロゲン化ブチルゴムのような官能基を付与した特殊グレードによらず、アセトニトリル、ジメチルスルフォキシド、メタノールのいずれの溶媒にも溶解度が３％以下となる。 In addition to regular rubber, halogenated butyl rubber can be used as the butyl rubber. These have a solubility of 3% or less in any solvent of acetonitrile, dimethyl sulfoxide, and methanol, regardless of the regular rubber grade by Mooney viscosity or the special grade to which a functional group is added such as halogenated butyl rubber.
また、粘着付与樹脂には、軟化点８５〜１４０℃の脂環族飽和炭化水素樹脂を使用できる。これらは軟化点の差等によるグレードによらずアセトニトリル、ジメチルスルフォキシド、メタノールのいずれの溶媒にも溶解度が３％以下となる。 Moreover, an alicyclic saturated hydrocarbon resin having a softening point of 85 to 140 ° C. can be used as the tackifier resin. These have a solubility of 3% or less in any solvent of acetonitrile, dimethyl sulfoxide and methanol regardless of the grade due to the difference in softening point.
また、上記ブチルゴム１００重量部に対して、上記脂環族飽和炭化水素樹脂５〜３０重量部を配合した粘着剤組成物も、アセトニトリル、ジメチルスルフォキシド、メタノールのいずれの溶媒にも溶解度が３％以下となる。 The pressure-sensitive adhesive composition in which 5 to 30 parts by weight of the alicyclic saturated hydrocarbon resin is blended with 100 parts by weight of the butyl rubber has a solubility of 3 in any solvent of acetonitrile, dimethyl sulfoxide, and methanol. % Or less.
また、上記粘着剤組成物をトルエンに溶解し、ポリエステルフィルムに塗布、乾燥することにより作製した本発明に係る粘着シート１は、マイクロプレートの成形に使用されるポリプロピレン、ポリスチレン、ポリカーボネートに対し十分に固定し得る３Ｎ／１０ｍｍ以上の粘着力を発揮することができる。 Moreover, the pressure-sensitive adhesive sheet 1 according to the present invention prepared by dissolving the pressure-sensitive adhesive composition in toluene, applying it to a polyester film and drying it is sufficient for polypropylene, polystyrene, and polycarbonate used for forming a microplate. An adhesive force of 3N / 10 mm or more that can be fixed can be exhibited.
上記脂環族飽和炭化水素樹脂の添加量は、５〜３０重量部が望ましい。上記脂環族飽和炭化水素樹脂の添加量が３０重量部を超えると、０℃において粘着力が低下し、十分に固定できる３Ｎ／１０ｍｍを下回る。また、添加量が５重量部未満の場合も粘着力が低下するからである。 The addition amount of the alicyclic saturated hydrocarbon resin is preferably 5 to 30 parts by weight. When the addition amount of the alicyclic saturated hydrocarbon resin exceeds 30 parts by weight, the adhesive strength is reduced at 0 ° C., which is less than 3 N / 10 mm which can be sufficiently fixed. This is also because the adhesive strength is reduced when the addition amount is less than 5 parts by weight.
また、本発明の粘着シート１の基材２としては、ポリエステルフィルムでは１０〜５０μｍの厚さ、ポリオレフィンフィルムでは２０〜１５０μｍの厚さ、および、それらプラスチックフィルムと５〜５０μｍの厚さのアルミ箔の複合体が好適であるが、マイクロプレートへの貼り付けを行う際に、極端に伸びたり、破れが発生することがなく、かつ、検査、分析時にシリンジ針が速やかに貫通し、針の折れ曲がり等が発生しない強度であることが必要な事項であり、この事項を満足できれば基材２の厚さは上記の範囲に限定されるものではない。
Moreover, as the
また、粘着剤層３はこれら基材２への密着力を十分に示すものであり、実用上支障をきたすことはないが、粘着シート１の製造時の都合や使用方法に合わせて密着力の改善が必要な場合は、基材２と粘着剤層３との間に、基材２の種類に合わせたアンカー剤層を設けたり、コロナ処理等の表面処理を行うことで密着力を改善することができる。
Further, the pressure-sensitive
［実施例１］
エクソン社製のレギュラーブチルゴム#０６５ １００ｇと、荒川化学社製の脂環族飽和炭化水素樹脂Ｐ−８５（軟化点８５℃）５ｇを、４２０ｇのトルエン中でミキサーにより溶解した。
[Example 1]
100 g of regular butyl rubber # 065 manufactured by Exxon Corporation and 5 g of alicyclic saturated hydrocarbon resin P-85 (softening point 85 ° C.) manufactured by Arakawa Chemical Co., Ltd. were dissolved in 420 g of toluene using a mixer.
その溶液を厚さ２５μｍのポリエステルフィルム上に、乾燥後の粘着剤層の厚さが４０μｍとなるように塗布し、１００℃で５分間の加熱により乾燥し、粘着シートを作製した。この際、ポリエステルフィルムと粘着剤層の密着力を得るため、ポリエステルにはコロナ処理を施した。
［実施例２］
エクソン社製のレギュラーブチルゴム#０６５ １００ｇと、荒川化学社製の脂環族飽和炭化水素樹脂Ｐ−１４０（軟化点１４０℃）５ｇを、４２０ｇのトルエン中でミキサーにより溶解した。
The solution was applied onto a 25 μm thick polyester film so that the thickness of the pressure-sensitive adhesive layer after drying was 40 μm, and dried by heating at 100 ° C. for 5 minutes to prepare a pressure-sensitive adhesive sheet. At this time, the polyester was subjected to corona treatment in order to obtain adhesion between the polyester film and the pressure-sensitive adhesive layer.
[Example 2]
100 g of regular butyl rubber # 065 manufactured by Exxon Corporation and 5 g of alicyclic saturated hydrocarbon resin P-140 (softening point 140 ° C.) manufactured by Arakawa Chemical Co., Ltd. were dissolved in 420 g of toluene using a mixer.
その溶液を厚さ２５μｍのポリエステルフィルム上に、乾燥後の粘着剤層の厚さが４０μｍとなるように塗布し、１００℃で５分間の加熱により乾燥し、粘着シートを作製した。この際、ポリエステルフィルムと粘着剤層の密着力を得るため、ポリエステルにはコロナ処理を施した。
［実施例３］
エクソン社製のレギュラーブチルゴム#０６５ １００ｇと、荒川化学社製の脂環族飽和炭化水素樹脂Ｐ−８５（軟化点８５℃）３０ｇを、５２０ｇのトルエン中でミキサーにより溶解した。
The solution was applied onto a 25 μm thick polyester film so that the thickness of the pressure-sensitive adhesive layer after drying was 40 μm, and dried by heating at 100 ° C. for 5 minutes to prepare a pressure-sensitive adhesive sheet. At this time, the polyester was subjected to corona treatment in order to obtain adhesion between the polyester film and the pressure-sensitive adhesive layer.
[Example 3]
100 g of regular butyl rubber # 065 manufactured by Exxon and 30 g of alicyclic saturated hydrocarbon resin P-85 (softening point 85 ° C.) manufactured by Arakawa Chemical Co., Ltd. were dissolved in 520 g of toluene using a mixer.
その溶液を厚さ２５μｍのポリエステルフィルム上に、乾燥後の粘着剤層の厚さが４０μｍとなるように塗布し、１００℃で５分間の加熱により乾燥し、粘着シートを作製した。この際、ポリエステルフィルムと粘着剤層の密着力を得るため、ポリエステルにはコロナ処理を施した。
［実施例４］
エクソン社製のレギュラーブチルゴム#０６５ １００ｇと、荒川化学社製の脂環族飽和炭化水素樹脂Ｐ−１４０（軟化点１４０℃）３０ｇを、５２０ｇのトルエン中でミキサーにより溶解した。
The solution was applied onto a 25 μm thick polyester film so that the thickness of the pressure-sensitive adhesive layer after drying was 40 μm, and dried by heating at 100 ° C. for 5 minutes to prepare a pressure-sensitive adhesive sheet. At this time, the polyester was subjected to corona treatment in order to obtain adhesion between the polyester film and the pressure-sensitive adhesive layer.
[Example 4]
100 g of regular butyl rubber # 065 manufactured by Exxon Corporation and 30 g of alicyclic saturated hydrocarbon resin P-140 (softening point 140 ° C.) manufactured by Arakawa Chemical Co., Ltd. were dissolved in 520 g of toluene using a mixer.
その溶液を厚さ２５μｍのポリエステルフィルム上に、乾燥後の粘着剤層の厚さが４０μｍとなるように塗布し、１００℃で５分間の加熱により乾燥し、粘着シートを作製した。この際、ポリエステルフィルムと粘着剤層の密着力を得るため、ポリエステルにはコロナ処理を施した。 The solution was applied onto a 25 μm thick polyester film so that the thickness of the pressure-sensitive adhesive layer after drying was 40 μm, and dried by heating at 100 ° C. for 5 minutes to prepare a pressure-sensitive adhesive sheet. At this time, the polyester was subjected to corona treatment in order to obtain adhesion between the polyester film and the pressure-sensitive adhesive layer.
溶解度の測定は、予め基材の重量（ａ）の分かっている粘着シートを、２０ｍｍ×５０ｍｍの寸法に切り出し、その重量（ｂ）を測定し、アセトニトリル、ジメチルスルフォキシド、メタノールの各溶媒５０ｍｌへ２４時間浸積し、１２０℃で２時間乾燥の後、室内で異物の付着がないように２４時間風乾したものの重量（ｃ）を測定した。 For the measurement of the solubility, an adhesive sheet whose weight (a) of the base material is known in advance is cut into a size of 20 mm × 50 mm, the weight (b) is measured, and each solvent of acetonitrile, dimethyl sulfoxide, and methanol is 50 ml. After being soaked for 24 hours and dried at 120 ° C. for 2 hours, the weight (c) of what was air-dried for 24 hours so that no foreign matter adhered in the room was measured.
測定した重量より、次式により溶解度を求め、溶解度が３％以下となるものを溶解しないと判断した。 From the measured weight, the solubility was determined by the following formula, and it was judged that the solution having a solubility of 3% or less was not dissolved.
溶解度（％）＝（ｃ−ｂ）／（ｂ−ａ）×１００
粘着力はＪＩＳ Ｚ ０２３７に準じて測定を行った。
Solubility (%) = (c−b) / (b−a) × 100
The adhesive strength was measured according to JIS Z 0237.
以下の表１に溶解度の測定結果およびシリコーン系粘着剤を使用した市販品との比較を、表２に溶解度の測定結果およびシリコーン系粘着剤を使用した市販品との比較を示す。
これら表１および表２からも分かるように市販品の溶解度は、最も少ないアセトニトリルでも５．５％であり、メタノールに至っては２６．５％という大きな値を示した。
Table 1 below shows the results of solubility measurement and comparison with commercial products using a silicone adhesive, and Table 2 shows results of solubility measurement and comparison with commercial products using a silicone adhesive.
As can be seen from Table 1 and Table 2, the solubility of the commercially available product was 5.5% even with the smallest acetonitrile, and a large value of 26.5% was reached for methanol.
これに対し、本発明に係る実施例は、アセトニトリル、ジメチルスルフォキシド、メタノールのいずれの溶媒にも溶解度が３％以下であった。また、本発明に係る実施例はいずれも０℃から４０℃の範囲で、ポリプロピレン・ポリスチレン・ポリカーボネートに対し３Ｎ／１０ｍｍ以上の高い粘着力が得られた。 On the other hand, the Examples according to the present invention had a solubility of 3% or less in any solvent of acetonitrile, dimethyl sulfoxide, and methanol. Further, in all of the examples according to the present invention, a high adhesive strength of 3 N / 10 mm or more was obtained with respect to polypropylene, polystyrene, and polycarbonate in the range of 0 ° C. to 40 ° C.
１…粘着シート
２…基材
３…粘着剤層
DESCRIPTION OF SYMBOLS 1 ...
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| JPH09165557A (en) * | 1995-12-15 | 1997-06-24 | Teraoka Seisakusho:Kk | Tacky tape for battery |
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