JP4428157B2 - Manufacturing method of laminate - Google Patents
Manufacturing method of laminate Download PDFInfo
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- JP4428157B2 JP4428157B2 JP2004195687A JP2004195687A JP4428157B2 JP 4428157 B2 JP4428157 B2 JP 4428157B2 JP 2004195687 A JP2004195687 A JP 2004195687A JP 2004195687 A JP2004195687 A JP 2004195687A JP 4428157 B2 JP4428157 B2 JP 4428157B2
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Description
本発明は、基材とポリオレフィン系樹脂層間の接着強度に優れ、包装材料に適した積層体の製造方法に関する。 The present invention relates to a method for producing a laminate that is excellent in adhesive strength between a base material and a polyolefin resin layer and is suitable for a packaging material.
ガスバリア性に優れた金属箔や金属蒸着フィルム、ポリエチレンテレフタレート（ＰＥＴ）やポリアミドなどの基材に対するポリオレフィン系樹脂の押出ラミネート成形は、食品や医療薬品などの包装を中心に広く採用されている方法である。従来、これらの基材と低密度ポリエチレンやポリプロピレンなどのポリオレフィン系樹脂との接着性を実用可能なレベルにまで高めるため、アンカーコート剤と称される接着促進剤を塗布する方法やポリオレフィン系樹脂をアクリル酸や無水マレイン酸などの不飽和カルボン酸で変性した変性ポリオレフィン系樹脂を用いる方法が採られていた。しかしながら、これらの方法は生産性やコストパフォーマンスに劣るため、改善が望まれていた。 Extrusion laminate molding of polyolefin resin to base materials such as metal foil and metal vapor-deposited film, polyethylene terephthalate (PET) and polyamide with excellent gas barrier properties is a widely adopted method mainly for packaging of food and medical chemicals. is there. Conventionally, in order to increase the adhesion between these base materials and polyolefin resins such as low density polyethylene and polypropylene to a practical level, a method of applying an adhesion promoter called an anchor coat agent or a polyolefin resin has been used. A method using a modified polyolefin resin modified with an unsaturated carboxylic acid such as acrylic acid or maleic anhydride has been adopted. However, since these methods are inferior in productivity and cost performance, improvement has been desired.
この改良方法として、押出ラミネート成形の際、溶融ポリオレフィン系樹脂にオゾンガスを吹付けた後、５０℃以上の温度で５分間以上熱処理する方法が提案されている（例えば、特許文献１参照）。また、ＰＥＴなどのプラスチック基材とポリオレフィン系樹脂の積層体を４０℃以上、または基材のガラス転移温度以上の温度で熱処理する方法が提案されている（例えば、特許文献２参照）。 As an improved method, a method of heat-treating at a temperature of 50 ° C. or more for 5 minutes or more after spraying ozone gas to the molten polyolefin-based resin during extrusion lamination molding has been proposed (for example, see Patent Document 1). In addition, a method has been proposed in which a laminate of a plastic substrate such as PET and a polyolefin resin is heat-treated at a temperature of 40 ° C. or higher or a glass transition temperature of the substrate or higher (for example, see Patent Document 2).
そこで、アンカーコート剤などの接着剤層を設けなくても、基材とポリオレフィン系樹脂との接着性に優れた積層体の製造方法が求められていた。 Therefore, there has been a demand for a method for producing a laminate having excellent adhesion between a substrate and a polyolefin resin without providing an adhesive layer such as an anchor coat agent.
本発明者らは、上記課題を解決すべく鋭意検討した結果、ポリオレフィン系樹脂を押出ラミネート法により積層した後に加圧下で加熱処理を行うことにより、アンカーコート剤などの接着剤層を設けなくても、基材とポリオレフィン系樹脂層とを強固に接着できることを見出し、本発明に至った。 As a result of intensive investigations to solve the above-mentioned problems, the present inventors have not provided an adhesive layer such as an anchor coat agent by performing a heat treatment under pressure after laminating a polyolefin resin by an extrusion laminating method. In addition, the present inventors have found that the base material and the polyolefin-based resin layer can be firmly bonded to each other and have reached the present invention.
すなわち、本発明は、押出ラミネート法により基材に接着剤層を介さずにポリオレフィン系樹脂を積層した後、０．１〜１．０ＭＰａで加圧しながら４０〜１４０℃の温度で熱処理することを特徴とする積層体の製造方法に関するものである。また、本発明は、前記ポリオレフィン系樹脂の押出成形温度が２６０〜３３０℃の範囲であり、かつ、基材と接するポリオレフィン系樹脂の表面をオゾン処理することを特徴とする積層体の製造方法に関するものであり、さらに、前記基材が、金属蒸着フィルムまたは金属箔であることを特徴とする積層体の製造方法に関するものである。 That is, in the present invention, after laminating a polyolefin resin on the base material without an adhesive layer by an extrusion laminating method, heat treatment is performed at a temperature of 40 to 140 ° C. while pressurizing at 0.1 to 1.0 MPa. It is related with the manufacturing method of the laminated body characterized. The present invention also relates to a method for producing a laminate, wherein the extrusion temperature of the polyolefin resin is in the range of 260 to 330 ° C., and the surface of the polyolefin resin in contact with the substrate is subjected to ozone treatment. Furthermore, the present invention relates to a method for producing a laminate, wherein the substrate is a metal vapor deposited film or a metal foil.
以下に、本発明について詳細に説明する。 The present invention is described in detail below.
本発明の積層体を構成する基材としては、金、銀、銅、鉄、アルミニウムなどの金属箔、金属蒸着フィルムなどの金属類、ポリエステル、ポリアミド、エチレン・酢酸ビニル共重合体鹸化物、エチレン・ビニルアルコール共重合体からなる群より選ばれる１種以上のフィルムまたはシートなどが挙げられる。これらの中でも各種金属蒸着フィルムやアルミ箔等の各種金属箔が好ましい。これらの基材の厚みには特に制限はなく、目的等に応じて適宜選定すればよいが、通常は５〜１００μｍ程度である。これらのラミネート用基材は、ラミネートするポリオレフィン系樹脂との接着性を向上させるために、必要に応じてコロナ放電処理や火炎処理等の表面処理を行なってもよい。 The base material constituting the laminate of the present invention includes metal foils such as gold, silver, copper, iron, and aluminum, metals such as metal vapor deposited films, polyester, polyamide, saponified ethylene / vinyl acetate copolymer, ethylene -One or more types of films or sheets selected from the group consisting of vinyl alcohol copolymers. Among these, various metal foils, such as various metal vapor deposition films and aluminum foil, are preferable. There is no restriction | limiting in particular in the thickness of these base materials, Although what is necessary is just to select suitably according to the objective etc., Usually, it is about 5-100 micrometers. These laminating base materials may be subjected to surface treatment such as corona discharge treatment or flame treatment as necessary in order to improve the adhesion to the polyolefin resin to be laminated.
本発明を構成するポリオレフィン系樹脂は、一般的にポリオレフィン系樹脂と称されているものでよく、このようなポリオレフィン系樹脂とは、エチレン、プロピレン、１−ブテンなどの炭素数２〜１２のα−オレフィンの単独重合体または共重合体を示す。例えば、低密度ポリエチレン、高密度ポリエチレン、エチレン・１−ブテン共重合体、エチレン・１−へキセン共重合体、エチレン・１−オクテン共重合体、エチレン・４−メチル−１−ペンテン共重合体などのエチレン・α−オレフィン共重合体；エチレン・アクリル酸共重合体、エチレン・メタクリル酸共重合体等のエチレン・アクリル酸共重合体；エチレン・アクリル酸エステル共重合体、エチレン・酢酸ビニル共重合体、エチレン・メタクリル酸エステル共重合体等のエチレン・ビニルエステル共重合体；ポリプロピレン、プロピレン・エチレン共重合体、プロピレン・１−ブテン共重合体などのプロピレン系重合体；、ポリ１−ブテン；ポリ１−ヘキセン；ポリ４−メチル−１−ペンテン等が挙げられ、これらポリオレフィン系樹脂は、一種単独または二種以上を組み合わせて用いてもよい。これらの中で、エチレン・α−オレフィン共重合体が熱処理後の接着性とコストパフォーマンスに優れるため好ましく、メタロセン触媒を用いて得られるエチレン・α−オレフィン共重合体が特に好ましい。 The polyolefin resin constituting the present invention may be generally called a polyolefin resin, and such a polyolefin resin is an α having 2 to 12 carbon atoms such as ethylene, propylene, 1-butene and the like. -Represents an olefin homopolymer or copolymer. For example, low density polyethylene, high density polyethylene, ethylene / 1-butene copolymer, ethylene / 1-hexene copolymer, ethylene / 1-octene copolymer, ethylene-4-methyl-1-pentene copolymer Such as ethylene / α-olefin copolymer; ethylene / acrylic acid copolymer, ethylene / acrylic acid copolymer such as ethylene / methacrylic acid copolymer; ethylene / acrylic acid ester copolymer, ethylene / vinyl acetate copolymer Polymers, ethylene / vinyl ester copolymers such as ethylene / methacrylic acid ester copolymers; propylene polymers such as polypropylene, propylene / ethylene copolymers, propylene / 1-butene copolymers; Poly 1-hexene, poly 4-methyl-1-pentene, and the like. It may be used in combination of at least one kind alone or in combination. Among these, an ethylene / α-olefin copolymer is preferable because of excellent adhesion and cost performance after heat treatment, and an ethylene / α-olefin copolymer obtained using a metallocene catalyst is particularly preferable.
本発明で用いるポリオレフィン系樹脂のＪＩＳ Ｋ６９２２−１（１９９８年）に従って測定した密度が８８０〜９１０ｋｇ／ｍ３の範囲であると基材との接着性に優れるため好ましい。 It is preferable that the density of the polyolefin resin used in the present invention measured in accordance with JIS K6922-1 (1998) is in the range of 880 to 910 kg / m 3 because of excellent adhesion to the substrate.
また、本発明で用いるポリオレフィン系樹脂のＪＩＳ Ｋ６９２２−１（１９９８年）に従って測定したメルトマスフローレートが５〜１００ｇ／１０分の範囲であると接着性に優れるため好ましい。 Moreover, since the melt mass flow rate measured according to JIS K6922-1 (1998) of the polyolefin resin used in the present invention is in the range of 5 to 100 g / 10 minutes, it is preferable because of excellent adhesiveness.
本発明で用いるポリオレフィン系樹脂の厚みは特に制限はなく、目的等に応じて適宜選定すればよいが、通常は１０〜２００μｍの範囲である。 The thickness of the polyolefin resin used in the present invention is not particularly limited and may be appropriately selected depending on the purpose and the like, but is usually in the range of 10 to 200 μm.
本発明で用いるポリオレフィン系樹脂は、押出ラミネート法により基材上に積層されて、ポリオレフィン系樹脂層を構成する。本発明における押出ラミネートとは、押出機を用いてポリオレフィン系樹脂を加熱、溶融し、ダイからフィルム状に押出して基材上に積層し、成形と貼り合わせを同時に行う成形方法である。ポリオレフィン系樹脂層は、基材の片面または両面にコートすることができる。さらに、本発明の押出ラミネート法には、二種類以上の樹脂を同時に押出す共押出ラミネート法や、二台の押出機を用いて順次コーティングするタンデムラミネート法が含まれる。 The polyolefin resin used in the present invention is laminated on a substrate by an extrusion laminating method to constitute a polyolefin resin layer. Extrusion lamination in the present invention is a molding method in which a polyolefin resin is heated and melted using an extruder, extruded from a die into a film, laminated on a substrate, and molding and bonding are performed simultaneously. The polyolefin resin layer can be coated on one side or both sides of the substrate. Furthermore, the extrusion laminating method of the present invention includes a coextrusion laminating method in which two or more kinds of resins are simultaneously extruded, and a tandem laminating method in which coating is performed sequentially using two extruders.
本発明において、加圧下における熱処理により接着強度を向上させるには、ポリオレフィン系樹脂を２６０〜３３０℃、好ましくは２８０〜３２０℃の温度範囲で成形することが好ましい。成形温度が低すぎると、成形後に加圧加熱処理を行っても接着強度が向上しない恐れがあり、成形温度が高すぎる場合には、成形時の発煙やヒートシール性などが悪化するため好ましくない。 In the present invention, in order to improve the adhesive strength by heat treatment under pressure, it is preferable to mold the polyolefin resin in a temperature range of 260 to 330 ° C, preferably 280 to 320 ° C. If the molding temperature is too low, the adhesive strength may not be improved even if pressure heating treatment is performed after molding, and if the molding temperature is too high, smoke generation or heat sealability during molding deteriorates, which is not preferable. .
また、押出されたポリオレフィン系樹脂に溶融状態でオゾン処理を施すことが好ましく、オゾン処理により、加圧下の熱処理による接着性改善効果が顕著になる。オゾンの吹付け量は、溶融ポリオレフィン系樹脂１ｍ２あたり０．１〜２００ｍｇが好適である。 Moreover, it is preferable to apply ozone treatment to the extruded polyolefin resin in a molten state, and the effect of improving adhesiveness by heat treatment under pressure becomes remarkable by ozone treatment. The amount of ozone sprayed is preferably 0.1 to 200 mg per 1 m 2 of the molten polyolefin resin.
本発明における加圧下の熱処理は、０．１〜１．０ＭＰａで加圧しながら４０〜１４０℃の温度で行うことを特徴とする。圧力が０．１ＭＰａ未満では接着性の改善効果が不十分であり、圧力が１．０ＭＰａを超える場合は積層体が変形するため好ましくない。また、温度が４０℃未満では接着性の改善効果が不十分であり、１４０℃を超える場合は積層体が変形するため好ましくない。このような処理方法としては、加熱した二本ロール間に積層体を通過させる方法や熱板によりプレスする方法などを例示することができる。また、加圧加熱時間は特に限定するものではないが、０．０１〜１０秒程度が生産性の点から好適である。 The heat treatment under pressure in the present invention is characterized by being performed at a temperature of 40 to 140 ° C. while pressurizing at 0.1 to 1.0 MPa. If the pressure is less than 0.1 MPa, the effect of improving the adhesiveness is insufficient, and if the pressure exceeds 1.0 MPa, the laminate is deformed, which is not preferable. Moreover, if the temperature is less than 40 ° C., the effect of improving adhesiveness is insufficient, and if it exceeds 140 ° C., the laminate is deformed, which is not preferable. Examples of such a processing method include a method of passing a laminate between heated two rolls, a method of pressing with a hot plate, and the like. Moreover, although pressurization heating time is not specifically limited, about 0.01 to 10 second is suitable from the point of productivity.
本発明の製造方法により、アンカーコート剤などの接着剤層を設けなくても、基材とポリオレフィン系樹脂との接着性に優れた積層体を得ることが可能である。 By the production method of the present invention, it is possible to obtain a laminate having excellent adhesion between the substrate and the polyolefin resin without providing an adhesive layer such as an anchor coating agent.
以下、実施例により本発明をさらに詳細に説明するが、本発明はこれら実施例に限定されるものではない。
（１）メルトマスフローレート（ＭＦＲ）
ＪＩＳ Ｋ６９２２−１（１９９８年）に準拠。
（２）密度
ＪＩＳ Ｋ６９２２−１（１９９８年）に準拠。
（３）基材との接着性
基材とポリオレフィン系樹脂組成物層間を剥離し、引張試験機（島津製作所（株）製、商品名オートグラフＤＣＳ５００）を用い、サンプル巾１５ｍｍ、剥離速度３００ｍｍ／分、１８０度剥離での剥離強度を測定し、該剥離強度を接着強度とした。
EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to these Examples.
(1) Melt mass flow rate (MFR)
Conforms to JIS K6922-1 (1998).
(2) Density Conforms to JIS K6922-1 (1998).
(3) Adhesiveness with base material The base material and the polyolefin-based resin composition layer are peeled, and using a tensile tester (manufactured by Shimadzu Corporation, trade name: Autograph DCS500), the sample width is 15 mm, the peeling speed is 300 mm / Minutes, the peel strength at 180 ° peel was measured, and the peel strength was defined as the adhesive strength.
実施例および比較例におけるポリオレフィン系樹脂としては、以下に示す二種類のポリエチレン［（Ｐ１），（Ｐ２）］を用いた。
（Ｐ１）高圧法低密度ポリエチレン（東ソー（株）製、商品名ペトロセン２０３、ＭＦＲ＝８ｇ／１０分、密度＝９１９ｋｇ／ｍ３）
（Ｐ２）エチレン・１−オクテン共重合体（ダウケミカル（株）製、商品名アフィニティ ＰＴ１４５０、ＭＦＲ＝８ｇ／１０分、密度＝９０２ｋｇ／ｍ３）
実施例１
ポリオレフィン系樹脂（Ｐ１）を９０ｍｍΦのスクリューを有する押出ラミネーターの押出機へ供給し、３２０℃の温度でＴダイ（開口長６００ｍｍ）より押出し、基材であるアルミ箔（住軽アルミ箔（株）製）と、サンドイッチ基材として厚み２５μｍの低密度ポリエチレンフィルムと厚み１２μｍのポリエチレンテレフタレートフィルムを予め積層した積層フィルム（以下、ＰＥ−ＰＥＴと記す。）との間に、成形速度１００ｍ／分で１５μｍの厚みとなるようにラミネートした。その後、圧縮成形機にて０．２ＭＰａの加圧下、１４０℃で１秒間熱処理を行い、アルミ箔／ポリオレフィン系樹脂／ＰＥ−ＰＥＴからなる積層体を得た。得られた積層体のアルミ箔とポリオレフィン系樹脂との間の接着強度を測定した。結果を表１に示す。
As the polyolefin resin in Examples and Comparative Examples, the following two types of polyethylene [(P1), (P2)] were used.
(P1) High-pressure method low-density polyethylene (trade name Petrocene 203, manufactured by Tosoh Corporation, MFR = 8 g / 10 min, density = 919 kg / m 3 )
(P2) Ethylene / 1-octene copolymer (manufactured by Dow Chemical Co., Ltd., trade name affinity PT1450, MFR = 8 g / 10 min, density = 902 kg / m 3 )
Example 1
The polyolefin resin (P1) is supplied to an extruder of an extrusion laminator having a 90 mmφ screw, extruded from a T die (opening length: 600 mm) at a temperature of 320 ° C., and an aluminum foil as a base material (Sumi Light Aluminum Foil Co., Ltd.) And a laminated film (hereinafter referred to as PE-PET) in which a low-density polyethylene film having a thickness of 25 μm and a polyethylene terephthalate film having a thickness of 12 μm are previously laminated as a sandwich substrate is 15 μm at a molding speed of 100 m / min. The laminate was laminated so as to have a thickness of. Then, it heat-processed for 1 second at 140 degreeC under the pressurization of 0.2 MPa with the compression molding machine, and obtained the laminated body which consists of aluminum foil / polyolefin-type resin / PE-PET. The adhesive strength between the aluminum foil of the obtained laminate and the polyolefin resin was measured. The results are shown in Table 1.
実施例２
圧縮成形機にて１４０℃、０．４ＭＰａの条件で加熱加圧処理を１秒間行う以外は、実施例１と同様の操作で積層体を得て、接着強度を測定した。結果を表１に示す。
Example 2
A laminate was obtained in the same manner as in Example 1 except that the heat and pressure treatment was performed for 1 second at 140 ° C. and 0.4 MPa in a compression molding machine, and the adhesive strength was measured. The results are shown in Table 1.
実施例３
ポリオレフィン系樹脂として（Ｐ２）を用い、押出温度を２８０℃とし、ポリエチレン溶融膜の接着面側にオゾン３０ｇ／ｍ３を含む空気を１時間あたり３ｍ３の流量で吹き付けて押出ラミネートする以外は実施例１と同様の操作で積層し、加熱加圧処理を行って積層体を得た。得られた積層体のアルミ箔とポリオレフィン系樹脂との間の接着強度を測定した。結果を表１に示す。
Example 3
(P2) is used as the polyolefin resin, the extrusion temperature is 280 ° C, and extrusion lamination is performed by blowing air containing ozone 30 g / m 3 at a flow rate of 3 m 3 per hour onto the adhesive surface of the polyethylene melt film. Lamination was performed in the same manner as in Example 1, and a heat and pressure treatment was performed to obtain a laminate. The adhesive strength between the aluminum foil of the obtained laminate and the polyolefin resin was measured. The results are shown in Table 1.
実施例４
厚み１２μｍのＰＥＴに、真空蒸着法により６００Åの厚みでアルミニウムを蒸着した基材を使用し、蒸着面側に実施例１と同様にポリオレフィン系樹脂層を押出ラミネート成形法により積層し、加熱加圧処理を行って積層体を得た。得られた積層体のアルミ箔とポリオレフィン系樹脂との間の接着強度を測定した。結果を表１に示す。
Example 4
Using a base material on which aluminum was deposited to a thickness of 600 mm by vacuum vapor deposition on PET with a thickness of 12 μm, a polyolefin-based resin layer was laminated on the vapor deposition surface side by extrusion laminating as in Example 1, and heated and pressurized The laminated body was obtained by processing. The adhesive strength between the aluminum foil of the obtained laminate and the polyolefin resin was measured. The results are shown in Table 1.
比較例１
実施例１においてラミネート成形後に加熱加圧処理を行わない以外は同様の方法で積層体を得た。得られた積層体の接着強度を測定した。結果を表１に示すが、接着性が劣っていた。
Comparative Example 1
A laminate was obtained in the same manner as in Example 1 except that the heat and pressure treatment was not performed after the laminate molding. The adhesive strength of the obtained laminate was measured. The results are shown in Table 1, but the adhesiveness was inferior.
比較例２
実施例１においてラミネート成形後に圧力を加えることなく加熱処理を行い積層体を得た。得られた積層体の接着強度を測定した。結果を表１に示すが、接着性が劣っていた。
Comparative Example 2
In Example 1, a heat treatment was performed without applying pressure after laminate molding to obtain a laminate. The adhesive strength of the obtained laminate was measured. The results are shown in Table 1, but the adhesiveness was inferior.
比較例３
実施例３においてラミネート成形後に加熱加圧処理を行わない以外は同様の方法で積層体を得た。得られた積層体の接着強度を測定した。結果を表１に示すが、接着性が劣っていた。
Comparative Example 3
A laminate was obtained in the same manner as in Example 3 except that the heat and pressure treatment was not performed after the laminate molding. The adhesive strength of the obtained laminate was measured. The results are shown in Table 1, but the adhesiveness was inferior.
比較例４
実施例４においてラミネート成形後に加熱加圧処理を行わない以外は同様の方法で積層体を得た。得られた積層体の接着強度を測定した。結果を表１に示すが、接着性が劣っていた。
Comparative Example 4
A laminate was obtained in the same manner as in Example 4 except that the heat and pressure treatment was not performed after the laminate molding. The adhesive strength of the obtained laminate was measured. The results are shown in Table 1, but the adhesiveness was inferior.
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| WO2013175693A1 (en) * | 2012-05-21 | 2013-11-28 | 三井化学株式会社 | Composite body and method for producing composite body |
| JP7450356B2 (en) * | 2018-09-28 | 2024-03-15 | 帝人株式会社 | Heat-modified polymer layer-inorganic base material composite, polymer member-inorganic base material composite, and manufacturing method thereof |
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| JPH0531850A (en) * | 1991-07-31 | 1993-02-09 | Mitsubishi Petrochem Co Ltd | Manufacture of aluminum laminated resin film |
| JPH1191051A (en) * | 1997-09-18 | 1999-04-06 | Nippon Polychem Kk | Laminate, resin or resin composition for forming laminate and method for treating the laminate |
| JP4410398B2 (en) * | 2000-07-05 | 2010-02-03 | 株式会社ジェイエスピー | Polypropylene resin foam sheet laminate and container |
| JP4945866B2 (en) * | 2001-08-29 | 2012-06-06 | 東ソー株式会社 | Ethylene-based resin composition for extrusion lamination, laminate using the same, and method for producing laminate |
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| CN110475655A (en) * | 2017-03-28 | 2019-11-19 | 电化株式会社 | The manufacturing method of laminated body, the manufacturing device of laminated body and laminated body |
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