JP2003171484A - Easily peelable film - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide an easily peelable film jointly equipped with a property for tightly sealing a content and an easily openable property both required for a packaging container, etc. <P>SOLUTION: This easily peelable film consists of 95-99.99 wt.% polyolefin- based resin and 0.01-5 wt.% compound having an epoxy group, containing 4-20% oxirane oxygen content obtained by a titration with hydrogen bromide and being liquid at 50°C, and is obtained by having an oxidation treatment on a surface to be heat-sealed. <P>COPYRIGHT: (C)2003,JPO

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to an easily peelable film. More specifically, the present invention relates to an easily peelable film having a sufficient seal strength for protecting the contents of a container and having an easy opening property, and its use.

[0002]

2. Description of the Related Art In a packaging container, it is easy to seal the contents and has a sealing strength that can be safely handled without breaking the bag during transportation. There is a demand for a sealant material that has an easy-open property so that it can be easily opened.

Examples of applications for such packaging containers are packaging bags for dry foods such as snacks, rice crackers, bonito flakes and frozen foods, pharmaceutical packaging bags for infusions, powdered medicines, granules, etc., yogurt and ice. Examples thereof include cup lid materials for creams, natto and the like, potion jelly and cup miso, cup lid materials for instant noodles and the like.

As the easily openable sealant material used for such a packaging bag and cup lid material, the following three types are generally mentioned according to the concept of the peeling mechanism of the sealant material which imparts the openability. .

1) A blend of a styrene / butadiene block copolymer mainly based on an ethylene / vinyl acetate copolymer (hereinafter referred to as EVA), or a tackifier such as a terpene resin to EVA. A type that uses a blended hot melt type that peels off at the interface between the adherend and the sealant material.

However, the sealant material called the interfacial peeling type exhibits easy opening property when the adherend is PP, PS, polyvinyl chloride, or polyester resin container, but in the case of polyethylene resin container. Easy opening is not obtained. Further, in the case where the adherend is a bag which seals the sealant materials, the easy opening property cannot be obtained.

2) A type in which the sealant material is formed of a multilayer film having two or more layers, and the seal interface between the adherend and the sealant material does not peel off when the seal is opened, but the layers of the sealant material peel off.

However, in this sealant material called the delamination type, since the innermost layer which becomes the sealing surface of the film remains on the adherend, the innermost layer thickness is made considerably thin in order to maintain a good peeling appearance. There must be. Therefore, it is necessary to use a co-extrusion film forming machine,
Coextrusion film formers are expensive and costly.

3) Polyethylene, EVA, and other polyethylene resins, polypropylene, polybutene, poly 4-methyl-1-pentene, and other poly α-olefins, polystyrene, styrene / butadiene block copolymers, ethylene / α-olefin copolymers. A type that uses a blend of united rubber and the sealant material itself undergoes cohesive failure and peels off.

However, this cohesive failure type sealant material can exhibit an easy-opening function when it becomes a seal between the sealant materials, but as a method of exhibiting the easy-opening property, a resin which is incompatible is blended. In order to
When melt-mixing the resin, the easy-open property changes due to the shear rate and shear stress. That is, there is a problem that it is difficult to obtain a stable product because it is affected by the film forming apparatus, the film forming temperature, the film forming speed, the film thickness, and the like. In order to reduce these problems, there is a method of adding a block copolymer or a graft copolymer as a compatibilizer, but the copolymer is very expensive and increases the cost of the sealant material. In addition, a so-called stringing phenomenon occurs in which the sealant material is broken into lines when peeling,
There is a problem that the peeling appearance is significantly impaired.

[0011]

SUMMARY OF THE INVENTION The present invention has been made in view of the above situation, and is directed to a seal between sealant materials, or to a component such as a container, a sheet, a multi-layer container or a multi-layer sheet, An easily peelable film that can be used as a sealant material that has easy peelability while maintaining sufficient heat-sealing strength to protect the contents, and that enables stable film formation, and that does not have a stringing phenomenon when the container is opened. And its purpose.

[0012]

Means for Solving the Problems As a result of intensive studies to solve the above problems, the present inventors have found that a polyolefin resin,
And a film made of a compound having a specific epoxy group, a seal between sealant materials, or a container, a sheet,
They have found that they are excellent as easily peelable sealant materials for components such as multilayer containers and multilayer sheets, and have completed the present invention.

That is, the present invention is a compound having 95 to 99.99% by weight of a polyolefin resin, an oxirane oxygen content of 4 to 20% as determined by titration with hydrogen bromide, and an epoxy group which is liquid at 50 ° C. The present invention relates to an easily peelable film, which comprises 0.01 to 5% by weight and whose surface to be heat-sealed is oxidized.

Further, in the present invention, it is preferable that the oxidation treatment is any one selected from corona discharge treatment, ozone treatment, flame treatment and plasma treatment.

The present invention also relates to an easily peelable film which is a multilayer film obtained by laminating the above easily peelable film as a heat seal layer.

Further, the present invention relates to an easily opened container characterized by comprising the above-mentioned easily peelable film, and in particular, the container is a bag.

Furthermore, the present invention is characterized in that the easily peelable film is a lid material for an easily openable container.

The present invention will be described in detail below.

The polyolefin resin constituting the easily peelable film of the present invention is a homopolymer or copolymer of an α-olefin having 2 to 12 carbon atoms such as ethylene, propylene and 1-butene. For example, high-pressure low-density polyethylene, high-density polyethylene, ethylene / 1-butene copolymer, ethylene / 1-hexene copolymer, ethylene / 1-octene copolymer, ethylene-4-methyl-1-
Ethylene type such as pentene copolymer, ethylene / vinyl acetate copolymer, ethylene / acrylic acid copolymer, ethylene / methacrylic acid copolymer, ethylene / acrylic acid ester copolymer, ethylene / methacrylic acid ester copolymer Polymers: polypropylene, propylene / ethylene copolymer, propylene / 1-butene copolymer, poly-1-butene, poly-1-hexene, poly-4-methyl-1-pentene, and the like. You may use it individually by 1 type or in combination of 2 or more types.

Preferably, the polyolefin resin used in the present invention is MFR according to JIS K6922-1.
Is in the range of 0.1 to 100 g / 10 min,
It is preferable because it is excellent in moldability when molding the easily peelable film.

The method for polymerizing the polyolefin resin used in the present invention is not particularly limited. In the case of high-pressure low-density polyethylene, ethylene / vinyl acetate copolymer, etc., for example, a radical polymerization method by a high-pressure method may be mentioned. And ethylene / 1-butene copolymer and ethylene / 1-
In the case of hexene copolymer, polypropylene, propylene / ethylene copolymer, poly 1-butene, etc., a polymerization method such as a gas phase method using a Ziegler-Natta catalyst or a metallocene catalyst, a solution method, a high pressure method and the like can be mentioned. .

The compound having an epoxy group constituting the easily peelable film of the present invention has an oxirane oxygen content of 4 to 20.
% (The oxirane oxygen content is determined by titration with hydrogen bromide as described in “Plasticizer—Theory and Application (Koshobo Publishing)”) and is characterized by a compound that is liquid at 50 ° C.

The oxirane oxygen content of the compound is 4 to 20%.
By this, the epoxy cross-linking density of the compound exuded on the film surface becomes appropriate and the easy peeling property is exhibited. Further, by being liquid at 50 ° C., the compound easily exudes onto the film surface, and the epoxy cross-linking reactivity on the film surface becomes easy.

The compound having an epoxy group constituting the easily peelable film of the present invention is not particularly limited, and epoxidized vegetable oil such as epoxidized soybean oil and epoxidized linseed oil; epoxidized polybutadiene (forming epoxidized polybutadiene) The polybutadiene to be used may be 1,2-polybutadiene or 1,4-polybutadiene), epoxidized polyisoprene, and the like.
Epoxidized soybean oil and epoxidized linseed oil are preferable, and epoxidized polybutadiene is particularly preferable.

The method of modifying the epoxy group-containing compound that constitutes the easily peelable film of the present invention is not particularly limited, but is described in JP-B-47-36271 and JP-B-51-31243. The illustrated method can be exemplified. Among these, a treatment method with a peracid is preferable in order to increase the amount of epoxy groups per molecule.

Examples of the epoxidized soybean oil include “Adeka Sizer O-130P” manufactured by Asahi Denka Kogyo, “Newsizer 510R” manufactured by NOF CORPORATION, “Kapox S-6” manufactured by Kao, and Asahi Denka Kogyo as epoxidized linseed oil. "Adeka Sizer O-180A" manufactured by Nippon Oil & Fats Co., Ltd. and "New Sizer 512" manufactured by NOF CORPORATION are exemplified, and examples of epoxidized polybutadiene include "Epolide RB3600" manufactured by Daicel Chemical Industries and "BF-1000" manufactured by Asahi Denka Kogyo.

The blending ratio of the polyolefin resin and the epoxy group-containing compound used in the present invention is 95 to 99.99% by weight of the polyolefin resin and 0.01 to 5% by weight of the epoxy group-containing compound.

When the compounding ratio of the compound having an epoxy group is less than 0.01% by weight, the easy-opening property is poor, and when it exceeds 5% by weight, the surface of the laminate obtained by extrusion laminating is sticky, Further, the cost becomes high, which is not preferable.

The easily peelable film of the present invention is characterized in that the surface to be heat-sealed is oxidized. By subjecting the film surface to an oxidation treatment, easy peeling property is exhibited.

This mechanism is such that, after the film is formed, the compound having an epoxy group leached on the film surface reacts with the oxide on the film surface to be immobilized on the polyolefin resin, and the oxide serves as a catalyst to form the polyolefin resin. This is because unreacted epoxy groups react with each other on the surface of the film to form a crosslinked structure, so that a part that becomes insoluble even by heat sealing is formed and heat sealing strength is optimized.

The oxidation treatment method is not particularly limited, and is not particularly limited, such as chromic acid treatment, sulfuric acid treatment, air oxidation, ozone treatment, corona discharge treatment, flame treatment and plasma treatment, but preferably ozone treatment, corona discharge treatment, Flame treatment and plasma treatment are good for effectively forming an oxide on the surface of the polyolefin resin.

The easily peelable film of the present invention may contain an additive that accelerates the curing reaction of the epoxy group. For example, aliphatic amines such as ethylenediamine, diethylenetriamine, triethylenetetramine and tetraethylenepentamine; aliphatic polyamines; aromatic amines such as diaminophenylsulfone and m-xylenediamine; primary amines such as pyridine, benzylmethylamine and triethanolamine. Tertiary amine; mercaptan type curing agent; phthalic anhydride,
Acid anhydrides such as maleic anhydride, trimellitic anhydride, hexahydrophthalic anhydride, tetrahydrophthalanol anhydride, hymic acid anhydride, and itaconic anhydride; fumaric acid, phthalic acid, maleic acid, trimellitic acid, adipic acid, sebacic acid And dicarboxylic acids such as dodecanedioic acid. You may use these as 1 type or a mixture of 2 or more types.

In addition, the easily peelable film of the present invention may optionally contain additives such as antioxidants, lubricants, neutralizing agents, antiblocking agents, surfactants and slip agents which are usually used for polyolefins. It doesn't matter what you do. The easily peelable film of the present invention is produced by an inflation molding machine, T
It can be obtained using a die cast molding machine, a calender molding machine, a press molding machine, or the like. Further, the easily peelable film obtained by these molding methods can be made into a multilayer film by sandwich laminating, dry laminating, thermal laminating, or the like, and various base materials can be formed by extrusion laminating or coextrusion laminating. It is also possible to melt-laminate the easily peelable film directly onto the above to obtain a multilayer film.

Examples of the above-mentioned substrate include synthetic polymer films and sheets, metal foils, papers, cellophane and the like. Among these, synthetic high molecular polymer films and sheets are particularly preferable, and examples thereof include films and sheets made of synthetic high molecular polymers such as polyethylene terephthalate, polyamide, polyvinyl alcohol, polycarbonate, polyethylene and polypropylene. Furthermore, these high molecular polymer films and sheets may be vapor-deposited with aluminum, vapor-deposited with alumina, or vapor-deposited with silicon dioxide. Further, these high molecular polymer films and sheets may be printed with urethane ink or the like.

Examples of the metal foil include aluminum foil and copper foil, and examples of the paper include kraft paper, high quality paper, glassine paper, cellophane and the like.

In addition, the easily peelable film obtained by the above-mentioned production method has a temperature of 30 ° C. or more in order to promote the exudation of the compound having an epoxy group to the film surface and the crosslinking reaction to develop a stable easy peeling property. It is preferable to age for 10 hours or more.

The thickness of the easily peelable film of the present invention is not particularly limited as long as the object of the present invention is achieved,
A thickness of 1 μm to 1 mm is preferable because it is excellent in flexibility and a problem such as breakage is small.

The easily peelable film of the present invention can be easily used as a container by hermetically sealing it with a heat seal. Examples of such a container include dried foods such as snacks, rice crackers, and bonito flakes. Bags for packaging frozen foods, bags for pharmaceuticals such as infusions, powders, and granules, yogurt and ice cream that are polyethylene laminated containers, lids for paper cups such as natto, potion jelly and cups PP for miso, improvised surface, etc.
It can be used as a lid material for containers, PS containers, PVC containers and the like.

[0039]

EXAMPLES The present invention will be described in more detail with reference to examples below, but the present invention is not limited to these examples.

The methods for measuring and evaluating the physical properties and workability are shown below.

(A) Melt mass flow rate (MFR) Conforms to JIS K6922-1.

(B) Density Conforms to JIS K6922-1.

(C) Assuming various uses of the easy-opening and easy-releasing film, the easily-releasing films obtained in the examples are (1) easy-releasing films, (2) easy-releasing film and high-pressure method. A low-density polyethylene sheet, and (3) an easily peelable film and a polypropylene sheet are superposed, and the pressure is 0.2 MPa and the time is 1
Second, heat sealing was performed by pressing with a heat sealing bar under the condition of a sealing temperature of 160 ° C. A sample width of 15 is applied to the heat-sealed portion using a tensile tester (manufactured by Shimadzu Corporation, trade name Autograph DCS500).
mm, peeling speed 300 mm / min, peeling strength at 180 ° peeling was measured, and the peeling strength was taken as heat seal strength and used as a measure of easy peelability.

(D) Appearance of unsealing The degree of the unsealed surface at the time of unsealing after heat sealing was evaluated, and those without stringing were indicated by ◯, and those with stringing were indicated by x.

Example 1 As a polyolefin resin, a high pressure low density polyethylene having a MFR of 8 g / 10 min and a density of 918 kg / m ³ (trade name: Petrosene 213, manufactured by Tosoh Corporation, hereinafter L)
It is written as DPE. ) 99.5% by weight, as a compound having an epoxy group, liquid epoxidized polybutadiene (trade name EPOLIDE RB3600 manufactured by Daicel Chemical Industries, Ltd.,
Hereinafter, it may be referred to as A) was blended so as to be 0.5% by weight and melt-kneaded with a single-screw extruder to obtain pellets.

The pellets thus obtained are fed to an extruder of an extrusion laminator having a 90 mmΦ screw, and 305
Extruded from T-die at a temperature of ℃, the thickness of the base material is 12 μm
Biaxially stretched polyester film (manufactured by Toyobo Co., Ltd.)
Product name Toyobo Ester Film E5100, hereinafter PET
Is written. ) And LDPE (Toso Co., Ltd. trade name Petrosene 213, thickness 25 μm), a two-layer film LDP
After laminating the easily peelable film on the E side so as to have a thickness of 30 μm, the surface of the easily peelable film was subjected to corona discharge treatment so as to be 50 W · min / m ² to obtain a multilayer easily peelable film.

The easily peelable film thus obtained was subjected to 40 hours for 40 hours.
After being stored in an oven kept at ℃, the easy peeling property was evaluated. The evaluation results are shown in Table 1.

Example 2 As a polyolefin resin, 99.5% by weight of LDPE (trade name Petrosene 213 manufactured by Tosoh Corporation) was used, and as a compound having an epoxy group, liquid epoxidized polybutadiene (trade name of Daicel Chemical Industries, Ltd.) was used. Epolide R
B3600) instead of 0.5 parts by weight, LDPE (Tosoh Corp. trade name Petrosene 213) 99% by weight,
1% by weight of liquid epoxidized polybutadiene (trade name EPOLIDE RB3600 manufactured by Daicel Chemical Industries, Ltd.)
An easily peelable film was obtained in the same manner as in Example 1 except for the above. The evaluation results are shown in Table 1.

Example 3 As a polyolefin resin, 99.5% by weight of LDPE (trade name: Petrosene 213, manufactured by Tosoh Corporation) was used, and a liquid epoxidized polybutadiene (trade name, manufactured by Daicel Chemical Industries, Ltd.) was used as a compound having an epoxy group. Epolide R
B3600) in place of 0.5 part by weight, 97% by weight of LDPE (trade name Petrosene 213 manufactured by Tosoh Corporation),
3% by weight of liquid epoxidized polybutadiene (manufactured by Daicel Chemical Industries, Ltd., trade name: Epolid RB3600)
An easily peelable film was obtained in the same manner as in Example 1 except for the above. The evaluation results are shown in Table 1.

Example 4 As a polyolefin resin, 99.5% by weight of LDPE (trade name Petrosene 213 manufactured by Tosoh Corporation) was used, and as a compound having an epoxy group, liquid epoxidized polybutadiene (trade name of Daicel Chemical Industries Ltd.) was used. Epolide R
B3600) instead of 0.5 part by weight, LDPE (Tosoh Corp. trade name Petrosene 213) 99.5 wt%, epoxidized soybean oil (Asahi Denka Kogyo brand name ADEKA CIZER O-130P, Hereinafter, it may be described as B.) An easily peelable film was obtained in the same manner as in Example 1 except that 0.5% by weight was used. The evaluation results are shown in Table 1.

Example 5 As a polyolefin resin, 99.5% by weight of LDPE (trade name: Petrosene 213, manufactured by Tosoh Corporation) was used, and a liquid epoxidized polybutadiene (trade name, manufactured by Daicel Chemical Industries, Ltd.) was used as a compound having an epoxy group. Epolide R
B3600) instead of 0.5 parts by weight, LDPE (Tosoh Corp. trade name Petrosene 213) 99% by weight,
An easily peelable film was obtained in the same manner as in Example 1 except that epoxidized soybean oil (Adeka Sizer O-130P, trade name, manufactured by Asahi Denka Kogyo Co., Ltd.) was changed to 1% by weight. The evaluation results are shown in Table 1.

Example 6 As a polyolefin resin, 99.5% by weight of LDPE (trade name: Petrosene 213, manufactured by Tosoh Corporation) was used, and a liquid epoxidized polybutadiene (trade name, manufactured by Daicel Chemical Industries, Ltd.) was used as a compound having an epoxy group. Epolide R
B3600, hereinafter sometimes referred to as A), instead of 0.5 part by weight, an ethylene / 1-hexene copolymer (manufactured by Tosoh Corp., trade name Nipolon-Z TZ420, hereinafter,
An easily peelable film was prepared in the same manner as in Example 1 except that 99.5% by weight of LLDPE) and 0.5% by weight of liquid epoxidized polybutadiene (trade name EPOLIDE RB3600 manufactured by Daicel Chemical Industries, Ltd.) were used. Obtained. The evaluation results are shown in Table 1.

Example 7 As a polyolefin resin, propylene-ethylene-1 having an MFR of 3 g / 10 minutes and a density of 900 kg / m ^3.
-Butene copolymer (manufactured by Chisso Corporation, trade name Chisso Polypro F8577, hereinafter referred to as PP) 99.5% by weight, as a compound having an epoxy group, liquid epoxidized polybutadiene (manufactured by Daicel Chemical Industries, Ltd.) 0.5% by weight of Eporide RB3600) was blended and melt-kneaded with a single-screw extruder to obtain pellets.

The obtained pellets were fed to an extruder of a T die cast molding machine having a screw of 50 mmΦ, and 2
It was extruded from a T-die at a temperature of 30 ° C. so as to have a thickness of 30 μm, and the surface of the film was subjected to corona discharge treatment so that the film had a thickness of 50 W · min / m ² to obtain an easily peelable film. The above-mentioned easily peelable film and PET as a base material having a thickness of 12 μm (trade name: Toyobo Ester Film E510, manufactured by Toyobo Co., Ltd.)
0) and a urethane adhesive (manufactured by Dainichiseika Co., Ltd., product side Seika Bond E-263 / C-26) were subjected to dry lamination molding to obtain a multilayer easily peelable film.

The easily peelable film obtained was 40 for 20 hours.
After being stored in an oven kept at ℃, the easy peeling property was evaluated. The evaluation results are shown in Table 1.

Example 8 Instead of subjecting the surface of the easily peelable film to corona discharge treatment so as to have a rate of 50 W · min / m ² , ozone gas was applied to the heat-sealed surface of the molten resin film extruded from the T-die.
Example 1 except that spraying was carried out so as to obtain mg / m ^2.
In the same manner as above, a multilayer easily peelable film was obtained, and the easy peelability was evaluated. The evaluation results are shown in Table 1.

[0057]

[Table 1] Comparative Example 1 99.5% by weight of LDPE (trade name Petrosene 213, manufactured by Tosoh Corporation) as a polyolefin resin, and liquid epoxidized polybutadiene (trade name EPOLIDE R manufactured by Daicel Chemical Industries, Ltd.) as a compound having an epoxy group.
B3600) 100 parts by weight of LDPE (Tosoh Corp. trade name Petrosene 213) instead of 0.5 parts by weight, and easy peelability in the same manner as in Example 1 except that a compound having an epoxy group was not used. I got a film. The evaluation results are shown in Table 2, but the heat seal strength was high and the easy peelability was not exhibited.

Comparative Example 2 99.5% by weight of LDPE (trade name Petrosene 213 manufactured by Tosoh Corporation) was used as a polyolefin resin, and liquid epoxidized polybutadiene (trade name of Daicel Chemical Industries, Ltd.) was used as a compound having an epoxy group. Epolide R
B3600) in place of 0.5 parts by weight, LDPE (Toso Co., Ltd. trade name Petrosene 213) 90% by weight,
An easily peelable film was obtained in the same manner as in Example 1 except that the amount of liquid epoxidized polybutadiene (trade name: Epolide RB3600 manufactured by Daicel Chemical Industries, Ltd.) was changed to 10% by weight. The evaluation results are shown in Table 2, but the film surface was sticky.

Comparative Example 3 Multilayer easy peeling was carried out in the same manner as in Example 1 except that corona discharge treatment was not performed in place of the corona discharge treatment so that the surface of the easily peelable film was 50 W · min / m ^2. To obtain a film. The evaluation results are shown in Table 2, but the heat seal strength was high and the easy peelability was not exhibited.

Comparative Example 4 As a polyolefin resin, 99.5% by weight of PP (trade name Chisso Polypro F8577 manufactured by Chisso Corporation) was used, and liquid epoxidized polybutadiene (manufactured by Daicel Chemical Industry Co., Ltd.) was used as a compound having an epoxy group. PP (Cisso Polypro F8577) 10 manufactured by Chisso Co., Ltd. instead of 0.5 parts by weight of Eporide RB3600)
An easily peelable film was obtained in the same manner as in Example 7 except that 0% by weight and the compound having an epoxy group were not used. The evaluation results are shown in Table 2, but the heat seal strength was high and the easy peelability was not exhibited.

[0061]

[Table 2]

EFFECT OF THE INVENTION The easily peelable film of the present invention has good easy peelability in sealing sealants with each other or with respect to containers and multi-layer containers to which polyethylene containers, polypropylene containers and the like are adhered. , A potion jelly, a confectionery, a cup miso, a tofu, a natto, an instant noodle, a frozen food, a retort food, and a sealant film suitable for packaging bags and containers.

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Claims (6)

[Claims] 1. A compound having an epoxy group, which is 95 to 99.99% by weight of a polyolefin resin, has an oxirane oxygen content of 4 to 20% as determined by titration with hydrogen bromide, and has a liquid epoxy group at 50 ° C. An easily peelable film comprising 5% by weight of which the surface to be heat-sealed is subjected to an oxidation treatment. 2. The easily peelable film according to claim 1, which is a multi-layer film in which the easily peelable film according to claim 1 is laminated as a heat seal layer. 3. The oxidation treatment according to claim 1, wherein the oxidation treatment is any one selected from corona discharge treatment, ozone treatment, flame treatment and plasma treatment. Easy peelable film. 4. An easy-open container comprising the easily peelable film according to claim 1 or 2. 5. An easily-openable bag comprising the easily peelable film according to claim 1 or 2. 6. A lid material for an easily openable container, comprising the easily peelable film according to claim 1 or 2.