JP4021059B2 - Manufacturing method of adhesive sheet - Google Patents
Manufacturing method of adhesive sheet Download PDFInfo
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- JP4021059B2 JP4021059B2 JP20518098A JP20518098A JP4021059B2 JP 4021059 B2 JP4021059 B2 JP 4021059B2 JP 20518098 A JP20518098 A JP 20518098A JP 20518098 A JP20518098 A JP 20518098A JP 4021059 B2 JP4021059 B2 JP 4021059B2
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- Japan
- Prior art keywords
- sheet
- pressure
- sensitive adhesive
- layer
- adhesive
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Description
【0001】
【発明の属する技術分野】
本発明は、屋外や屋内でマーキングや装飾用として用いられ、基材シートと粘着剤層との密着性にすぐれた粘着シートの製造方法に関する。
【0002】
【従来の技術】
従来より基材シートに粘着剤層が積層された粘着テープもしくはシートにおいて、基材シートと粘着剤層との界面接着力(以下アンカー力という)を向上させるための検討が進められてきた。このアンカー力が低いと被着体に貼り付けた粘着テープもしくはシートを剥がすとき、基材シートから粘着剤層が剥離して被着体に接着したまま残される(糊残りという)。特にマーキングや装飾用では用済み後に剥がすことが頻繁に行われるため、糊残りは粘着テープもしくはシートの品質上大きな問題とされている。
【0003】
特に基材シートが塩化ビニル系樹脂である場合には、熱安定剤として通常使用されている金属石鹸系熱安定剤がフィルム成形後に基材シート表面と粘着剤層との界面にブリードアウトし、粘着剤層とのアンカー力を低下させるという問題がある。
【0004】
基材シートと粘着剤層との接着性を向上させるために、基材シートにアンカー剤を塗布することが知られている。例えば、特開昭51−91944号公報には2液型の積層フィルム用アンカー剤が開示されている。このものは限られた状況において充分なアンカー性能を発揮するが、上記の金属石鹸等がブリードアウトして界面に薄膜層を形成しているような場合にはアンカー力が発揮されないという問題点があった。
【0005】
【発明が解決しようとする課題】
本発明は上記の問題点を解消し、基材シート表面に金属石鹸成分がブリードアウトしていてもアンカー力が低下することがなく、被着体から剥離しても糊残りが発生しない粘着シートの製造方法を提供することを目的とする。
【0006】
【課題を解決するための手段】
本発明の粘着シートの製造方法は、アクリロニトリル−メチルメタクリレート共重合体及び分子内にカルボキシル基を有するアクリロニトリル−ブタジエン共重合体からなる樹脂成分と、水と任意に混合可能な有機溶剤または該有機溶剤と水との混合溶剤よりなるプライマー溶液を乾燥後の厚みが0.05〜3μmとなるように合成樹脂シートの一面に塗布乾燥してプライマー層を形成し、次いで該プライマー層面に粘着剤層を積層することを特徴とする。
【0007】
分子内にカルボキシル基を有するアクリロニトリル−ブタジエン共重合体を得るには、アクリロニトリルとブタジエンを共重合させてブタジエンに由来する二重結合部分にカルボキシル基を導入する方法が一般的であるが、これに限定されるものではない。分子内にカルボキシル基が導入されていることによりアンカー力が向上する。
【0008】
アクリロニトリル−メチルメタクリレート共重合体(以下、共重合体Aという)と上記分子内にカルボキシル基を有するアクリロニトリル−ブタジエン共重合体(以下、共重合体Bという)とを混合することにより、アンカー力及び柔軟性が向上し、界面剥離し難くなる。
【0009】
共重合体Aと共重合体Bとの混合比率は、共重合体Aが多くなるとガラス転移温度が高くなって界面剥離が起こり易くなり、共重合体Bが多くなると合成樹脂シートとしてオレフィン系樹脂を使用した場合にアンカー力が得られなくなるため、A:Bは20:80〜80:20が好ましく、より好ましくは30:70〜70:30である。
【0010】
有機溶剤は水と任意に混合可能なものであればよく、炭素数4以下のアルキル基を有するアルコール類、アセトンなどが挙げられる。炭素数4以下のアルキル基を有するアルコール類としては、メタノール、エタノール、イソプロパノール、ブタノールなどが挙げられる。
【0011】
上記有機溶剤と水との量関係は、有機溶剤が多くなるとコストが高くなり経済的に不利になることがあり、水が多くなると乾燥のために多大のエネルギーと時間を要するので、有機溶剤と水との混合比率は100:0〜30:70が好ましく、より好ましくは70:30〜35:65である。
【0012】
このような有機溶剤または有機溶剤と水との混合溶剤は、合成樹脂シート表面にブリードアウトしている金属石鹸を溶解除去し、プライマー層と合成樹脂シート表面との接着力を高める。ここで金属石鹸成分を溶解除去するとは界面に薄膜層を形成させないという意味であり、金属石鹸成分は薄膜層を形成せずプライマー層内に溶解または分散されるものと考えられる。
【0013】
本発明で使用される合成樹脂シートとしては、低密度ポリエチレン、高密度ポリエチレン、直鎖状低密度ポリエチレンなどのエチレン系樹脂、プロピレン系樹脂、塩化ビニル系樹脂などのシートが用いられる。塩化ビニル系樹脂シートの場合では、カレンダー成形、キャスティング成形のいずれの成形法によるものでもよい。
【0014】
上記樹脂成分と溶剤成分とからなるプライマー溶液を合成樹脂シートの粘着剤層を積層する面に直接塗布して乾燥させる。プライマー層の厚みは乾燥後で0.05〜3μmとなるように設定する。この厚みが0.05μm未満であるとアンカー効果が不充分となり、3μmを超えると着色が現れることがあり、また、乾燥速度が遅くなることもある。更に、コスト面で不利である。
【0015】
【発明の実施の形態】
(実施例1〜8;比較例1〜7)
塩化ビニル系樹脂(重合度1200)100重量部に対して、可塑剤(旭電化社製,商品名「PN250」)30重量部、希釈溶剤(キシレン)100重量部、ベンゾトリアゾール系紫外線吸収剤(チバガイギー社製,商品名「チヌビンP」)1重量部、顔料(キナクリンレッド)5重量部、Ba−Zn金属石鹸系熱安定剤(勝田加工社製,商品名「BZ180」)4重量部を配合した塩化ビニル系樹脂分散溶液を、厚み75μmの片面離型処理したフィルムの処理面に塗工し、200℃で5分間加熱処理して厚み50μmの塩化ビニル系樹脂シートを作製した。
【0016】
次に、表1および表2の配合組成に従って調製したプライマー溶液を、上記塩化ビニル系樹脂シートの一面に塗布乾燥することにより、プライマー層を積層した塩化ビニル系樹脂シートを得た。但し、比較例7ではプライマー溶液を塗布しなかった。
別途、上質紙の両面にポリエチレンをラミネートした離型紙にアクリル粘着剤(綜研化学社製,商品名「SK1335」)100重量部に架橋剤(綜研化学社製,M−5A)5重量部を配合したものを攪拌後塗布し、乾燥後の厚みが30μmの粘着剤層を形成した。
上記粘着剤層を40℃の条件下で上記シートのプライマー層積層面に貼り合わせて粘着シートを得た。
【0017】
性能評価
上記実施例1〜8及び比較例1〜7で得られた粘着シートに関し、以下の項目について評価し、その結果を表1および表2に示した。
(1)プライマー層の初期着色の有無
上記粘着シートを透明なアクリル樹脂板に貼付し、粘着シート貼付面とは反対 面から目視で観察し、着色の有無を評価した。
【0018】
(2)アンカー力
厚さ50μmのポリエチレンテレフタレートフィルムの一面に下塗り剤(日本触媒社製,商品名「ポリメントNK−350」)を1μmの厚さで塗布した試験用フィルムの下塗り剤塗布面に、25mm×100mmにカットした各粘着シートを2kgの圧着ローラーを2往復させることにより貼付し、110℃のオーブン中で1時間養生し、23℃恒温室中で2時間静置することによりサンプルを得た。
次いで、図1に示したように塩化ビニル系樹脂シート3の一端を剥離し、ポリエチレンテレフタレートフィルム1と粘着剤層2を180°方向に引き剥がすことによりT型剥離試験を行い、塩化ビニル系樹脂シート3と粘着剤層2とのアンカー力を測定した。
【0019】
(3)SUS板への糊残り
SUS#304の試験板(サイズ50mm×120mm)に、25mm×100mmにカットした各粘着シートを、2kgの圧着ローラーを2往復させることにより貼付し、23℃恒温室内で24時間放置し、養生した。
次いで、人手により高速剥離した際の試験板への糊残りを下記の評価基準に従って評価した。
(評価基準)
5:糊残りなし
4:糊残り10%未満
3:糊残り20%未満
2:糊残り50%未満
1:糊残り50%以上
【0020】
(4)耐候性
アルミニウム板(サイズ20mm×35mm)に、同一サイズにカットした各粘着シートを、2kgの圧着ローラーを2往復させることにより貼付した。
次いで、サンシャインウエザオメーター(スガ試験機社製,商品名「ウエザオメーターWEL−SUN−HC」)内に設置し、紫外線を3000時間照射した後の退色の度合いを、初期値との差として色差計(ミノルタ社製,装置名「分光測色計CM3700d」)を用いて測定した。
【0021】
【表1】
【0022】
【表2】
【0023】
表1及び表2から明らかなように、実施例1〜8のものは比較例1〜3及び比較例5〜7のものに比べ、アンカー力が飛躍的に大きくなり、他の評価もすべて満足な結果が得られた。比較例4のものはアンカー力は大きいがプライマー層の厚みが大きいので初期着色が著しく現れた。
【0024】
【発明の効果】
本発明の粘着シートの製造方法によると、基材シート表面に金属石鹸成分がブリードアウトしていても合成樹脂シートに対する粘着剤層のアンカー力が低下しないので被着体から剥離しても糊残りが発生せず、着色のない優れた外観を有する粘着シートを得ることができる。
【図面の簡単な説明】
【図1】アンカー力を測定する状態を示す断面図。
【符号の説明】
1:ポリエチレンテレフタレートフィルム
2:粘着剤層
3:塩化ビニル系樹脂シート[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing a pressure-sensitive adhesive sheet that is used for marking or decoration outdoors or indoors and has excellent adhesion between a substrate sheet and a pressure-sensitive adhesive layer.
[0002]
[Prior art]
Conventionally, studies have been made to improve the interfacial adhesive force (hereinafter referred to as anchor force) between a base sheet and an adhesive layer in an adhesive tape or sheet in which an adhesive layer is laminated on a base sheet. When the anchor force is low, when the adhesive tape or sheet attached to the adherend is peeled off, the adhesive layer is peeled off from the base sheet and remains adhered to the adherend (referred to as adhesive residue). Especially for marking and decorative purposes, peeling off after use is frequently performed, so that the adhesive residue is a serious problem in terms of the quality of the adhesive tape or sheet.
[0003]
In particular, when the base sheet is a vinyl chloride resin, a metal soap heat stabilizer usually used as a heat stabilizer bleeds out to the interface between the base sheet surface and the adhesive layer after film formation, There exists a problem of reducing the anchor force with an adhesive layer.
[0004]
In order to improve the adhesion between the base sheet and the pressure-sensitive adhesive layer, it is known to apply an anchor agent to the base sheet. For example, Japanese Patent Application Laid-Open No. 51-91944 discloses a two-component type anchor agent for laminated film. This product exhibits sufficient anchor performance in a limited situation, but there is a problem that the anchor force is not exhibited when the above metal soap or the like bleeds out to form a thin film layer at the interface. there were.
[0005]
[Problems to be solved by the invention]
The present invention eliminates the above-mentioned problems, and the adhesive force does not decrease even if the metal soap component bleeds out on the surface of the base sheet, and no adhesive residue is generated even if it is peeled off from the adherend. It aims at providing the manufacturing method of.
[0006]
[Means for Solving the Problems]
The method for producing a pressure-sensitive adhesive sheet of the present invention comprises a resin component comprising an acrylonitrile-methyl methacrylate copolymer and an acrylonitrile-butadiene copolymer having a carboxyl group in the molecule, an organic solvent optionally mixed with water, or the organic solvent A primer solution composed of a mixed solvent of water and water is applied to one surface of a synthetic resin sheet so as to have a thickness after drying of 0.05 to 3 μm to form a primer layer, and then an adhesive layer is formed on the primer layer surface. It is characterized by being laminated.
[0007]
In order to obtain an acrylonitrile-butadiene copolymer having a carboxyl group in the molecule, a method in which acrylonitrile and butadiene are copolymerized to introduce a carboxyl group into a double bond portion derived from butadiene is generally used. It is not limited. Anchor force is improved by introducing a carboxyl group into the molecule.
[0008]
By mixing an acrylonitrile-methyl methacrylate copolymer (hereinafter referred to as copolymer A) and an acrylonitrile-butadiene copolymer having a carboxyl group in the molecule (hereinafter referred to as copolymer B), anchor strength and Flexibility is improved and interfacial peeling is difficult.
[0009]
The mixing ratio of the copolymer A and the copolymer B is such that when the amount of the copolymer A increases, the glass transition temperature becomes high and interfacial peeling easily occurs. When the amount of the copolymer B increases, an olefin resin as a synthetic resin sheet When A is used, the anchor force cannot be obtained, so A: B is preferably 20:80 to 80:20, more preferably 30:70 to 70:30.
[0010]
The organic solvent may be any solvent that can be arbitrarily mixed with water, and examples thereof include alcohols having an alkyl group having 4 or less carbon atoms and acetone. Examples of the alcohol having an alkyl group having 4 or less carbon atoms include methanol, ethanol, isopropanol, and butanol.
[0011]
The quantity relationship between the organic solvent and water is that the cost increases and the economy becomes disadvantageous when the amount of the organic solvent increases, and when the amount of water increases, it takes a lot of energy and time for drying. The mixing ratio with water is preferably 100: 0 to 30:70, more preferably 70:30 to 35:65.
[0012]
Such an organic solvent or a mixed solvent of an organic solvent and water dissolves and removes the metal soap that bleeds out on the surface of the synthetic resin sheet, and increases the adhesion between the primer layer and the surface of the synthetic resin sheet. Here, dissolving and removing the metal soap component means that a thin film layer is not formed at the interface, and the metal soap component is considered to be dissolved or dispersed in the primer layer without forming the thin film layer.
[0013]
Examples of the synthetic resin sheet used in the present invention include sheets of ethylene resins such as low density polyethylene, high density polyethylene, and linear low density polyethylene, propylene resins, and vinyl chloride resins. In the case of a vinyl chloride resin sheet, it may be formed by either a calendar molding or a casting molding.
[0014]
The primer solution composed of the resin component and the solvent component is directly applied to the surface of the synthetic resin sheet on which the adhesive layer is laminated and dried. The thickness of the primer layer is set to 0.05 to 3 μm after drying. If the thickness is less than 0.05 μm, the anchor effect is insufficient, and if it exceeds 3 μm, coloring may appear, and the drying speed may be slow. Furthermore, it is disadvantageous in terms of cost.
[0015]
DETAILED DESCRIPTION OF THE INVENTION
(Examples 1-8; Comparative Examples 1-7)
100 parts by weight of a vinyl chloride resin (degree of polymerization 1200), 30 parts by weight of a plasticizer (trade name “PN250” manufactured by Asahi Denka Co., Ltd.), 100 parts by weight of a diluting solvent (xylene), a benzotriazole ultraviolet absorber ( 1 part by weight of Ciba Geigy Co., Ltd., trade name “Tinubin P”), 5 parts by weight of pigment (quinacrine red), 4 parts by weight of Ba—Zn metal soap heat stabilizer (trade name “BZ180”, manufactured by Katsuta Processing Co., Ltd.) The vinyl chloride resin dispersion solution thus applied was applied to the treated surface of a film having a single-sided release treatment with a thickness of 75 μm and heat-treated at 200 ° C. for 5 minutes to prepare a vinyl chloride resin sheet with a thickness of 50 μm.
[0016]
Next, the primer solution prepared according to the composition of Table 1 and Table 2 was applied and dried on one surface of the vinyl chloride resin sheet to obtain a vinyl chloride resin sheet having a primer layer laminated thereon. However, in Comparative Example 7, the primer solution was not applied.
Separately, 100 parts by weight of an acrylic adhesive (trade name “SK1335”, manufactured by Soken Chemical Co., Ltd.) and 5 parts by weight of a cross-linking agent (manufactured by Soken Chemical Co., Ltd., M-5A) are mixed with release paper in which polyethylene is laminated on both sides of fine paper. This was applied after stirring to form an adhesive layer having a thickness of 30 μm after drying.
The pressure-sensitive adhesive layer was bonded to the primer layer lamination surface of the sheet at 40 ° C. to obtain a pressure-sensitive adhesive sheet.
[0017]
Performance Evaluation Regarding the pressure-sensitive adhesive sheets obtained in Examples 1 to 8 and Comparative Examples 1 to 7, the following items were evaluated, and the results are shown in Tables 1 and 2.
(1) Presence or absence of initial coloring of primer layer The pressure-sensitive adhesive sheet was affixed to a transparent acrylic resin plate and visually observed from the side opposite to the surface where the pressure-sensitive adhesive sheet was applied to evaluate the presence or absence of coloring.
[0018]
(2) An undercoating agent applied to a surface of a polyethylene terephthalate film having an anchoring force thickness of 50 μm with an undercoat agent (trade name “Polyment NK-350” manufactured by Nippon Shokubai Co., Ltd.) with a thickness of 1 μm. Each adhesive sheet cut to 25mm x 100mm was pasted by reciprocating 2kg pressure roller twice, cured in 110 ° C oven for 1 hour, and left in 23 ° C constant temperature room for 2 hours to obtain sample It was.
Next, as shown in FIG. 1, one end of the vinyl chloride resin sheet 3 is peeled off, and a T-type peel test is performed by peeling the
[0019]
(3) Adhesive residue on SUS plate Each adhesive sheet cut to 25 mm x 100 mm was pasted on a test plate of SUS # 304 (size 50 mm x 120 mm) by reciprocating two 2 kg pressure rollers, and kept at a constant temperature of 23 ° C. It was left indoors for 24 hours and cured.
Next, the adhesive residue on the test plate when peeled at high speed manually was evaluated according to the following evaluation criteria.
(Evaluation criteria)
5: No adhesive residue 4: Less than 10% adhesive residue 3: Less than 20% adhesive residue 2: Less than 50% adhesive residue 1: More than 50% adhesive residue
(4) Each pressure-sensitive adhesive sheet cut to the same size was attached to a weather-resistant aluminum plate (size 20 mm × 35 mm) by reciprocating a 2 kg pressure roller twice.
Next, the degree of fading after being installed in a sunshine weatherometer (trade name “Weatherometer WEL-SUN-HC” manufactured by Suga Test Instruments Co., Ltd.) and irradiated with ultraviolet rays for 3000 hours is defined as the difference from the initial value. Measurement was performed using a color difference meter (manufactured by Minolta Co., Ltd., apparatus name “spectral colorimeter CM3700d”).
[0021]
[Table 1]
[0022]
[Table 2]
[0023]
As is clear from Tables 1 and 2, the anchors of Examples 1 to 8 are dramatically larger than those of Comparative Examples 1 to 3 and Comparative Examples 5 to 7, and all other evaluations are satisfied. Results were obtained. Although the thing of the comparative example 4 had large anchor force, since the thickness of the primer layer was large, initial coloring appeared remarkably.
[0024]
【The invention's effect】
According to the method for producing a pressure-sensitive adhesive sheet of the present invention, even if the metal soap component bleeds out on the surface of the base material sheet, the anchor force of the pressure-sensitive adhesive layer with respect to the synthetic resin sheet does not decrease. It is possible to obtain a pressure-sensitive adhesive sheet having no appearance and no coloring.
[Brief description of the drawings]
FIG. 1 is a cross-sectional view showing a state in which anchor force is measured.
[Explanation of symbols]
1: Polyethylene terephthalate film 2: Adhesive layer 3: Vinyl chloride resin sheet
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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JP20518098A JP4021059B2 (en) | 1998-07-21 | 1998-07-21 | Manufacturing method of adhesive sheet |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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JP20518098A JP4021059B2 (en) | 1998-07-21 | 1998-07-21 | Manufacturing method of adhesive sheet |
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JP2000034448A JP2000034448A (en) | 2000-02-02 |
JP4021059B2 true JP4021059B2 (en) | 2007-12-12 |
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JP20518098A Expired - Lifetime JP4021059B2 (en) | 1998-07-21 | 1998-07-21 | Manufacturing method of adhesive sheet |
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JP6265862B2 (en) | 2013-09-17 | 2018-01-24 | 株式会社パックス | Packaging container and manufacturing method thereof |
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1998
- 1998-07-21 JP JP20518098A patent/JP4021059B2/en not_active Expired - Lifetime
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