JP2016069441A - Layered silicate-containing resin composition, and resin molded article obtained by using the same - Google Patents
Layered silicate-containing resin composition, and resin molded article obtained by using the same Download PDFInfo
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本発明は層状ケイ酸塩が均一分散した樹脂組成物およびこれを用いて得られる樹脂成形品に関するものである。 The present invention relates to a resin composition in which layered silicate is uniformly dispersed and a resin molded product obtained using the same.
ナノサイズのフィラーはそのもの自体が特殊な性質を有する場合があり、これをコンポジット化することで優れた複合材料とする研究が多くなされている。ナノサイズのフィラーの中でも、層状ケイ酸塩は板状でありかつ層状であるため、完全に層剥離させた場合においては、個々のアスペクト比が高いことからさらに物性への影響を与えやすい。特に高分子材料とのコンポジット化は、引張強さの増大、弾性率の増大、耐熱性の向上、難燃性の向上、ガスバリア性の向上などさまざまな利点があり、工業上の価値があるとされている。
しかしながら、層状ケイ酸塩と高分子材料のコンポジット化は、層状ケイ酸塩自体が親水性であることから、両者の界面自由エネルギーの差が大きく、そのまま混合すると分散性が悪い。層状ケイ酸塩の分散性を向上させるためには種々の工夫がなされており、例えば、層状ケイ酸塩を有機シラン化合物で表面処理したものを高分子材料と溶融混錬することが知られている（例えば特許文献１等）。
Nano-sized fillers themselves may have special properties, and many studies have been made to make them excellent composite materials by compositing them. Among the nano-sized fillers, the layered silicate is plate-like and layered, and therefore, when completely delaminated, the individual aspect ratio is high, and thus the physical properties are more easily affected. In particular, compositing with polymer materials has various advantages such as increased tensile strength, increased elastic modulus, improved heat resistance, improved flame retardancy, and improved gas barrier properties, and has industrial value. Has been.
However, when the layered silicate and the polymer material are made into a composite, since the layered silicate itself is hydrophilic, the difference in interfacial free energy between the two is large, and when mixed as they are, the dispersibility is poor. Various improvements have been made to improve the dispersibility of the layered silicate. For example, it is known that a layered silicate surface-treated with an organosilane compound is melt-kneaded with a polymer material. (For example, Patent Document 1).
しかしながら、このような表面処理した層状ケイ酸塩を溶融混錬しても、高分子材料中における分散性は未だ十分とは言えず、さらなる改善が望まれていた。 However, even if such a surface-treated layered silicate is melt-kneaded, the dispersibility in the polymer material is still not sufficient, and further improvement has been desired.
本発明は、斯かる事情を考慮しなされたものであり、層状ケイ酸塩を高分子材料中に均一に分散させることを目的に種々検討したところ、高分子材料として特定の酸含有量のエチレン−酢酸ビニル共重合体を用い、当該エチレン−酢酸ビニル共重合体に層状ケイ酸塩を添加することで、層状ケイ酸塩を均一分散させることが可能であることを見出し、完成させたものである。よって本発明は、以下を要旨とする。
（１）酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩を１〜２０重量％含有してなることを特徴とする層状ケイ酸塩を含有してなる樹脂組成物。
（２）（１）に記載の樹脂組成物からなる樹脂成形品。
（３）（１）に記載の樹脂組成物と、他の合成樹脂とを含有してなる樹脂成形品。
The present invention has been made in view of such circumstances, and various studies have been made for the purpose of uniformly dispersing the layered silicate in the polymer material. As a polymer material, ethylene having a specific acid content has been obtained. -A vinyl acetate copolymer was used, and it was found that the layered silicate can be uniformly dispersed by adding a layered silicate to the ethylene-vinyl acetate copolymer. is there. Therefore, this invention makes the following a summary.
(1) A resin comprising a layered silicate, wherein the ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more contains 1 to 20% by weight of a layered silicate. Composition.
(2) A resin molded product comprising the resin composition according to (1).
(3) A resin molded product comprising the resin composition according to (1) and another synthetic resin.
本発明の樹脂組成物は、合成樹脂中に層状ケイ酸塩が均一分散してなるものである。そのため、当該樹脂組成物を用いて得られる樹脂成形品は、引張強さの増大、弾性率の増大、耐熱性の向上、難燃性の向上、ガスバリア性の向上などさまざまな利点を有するものである。 The resin composition of the present invention is obtained by uniformly dispersing a layered silicate in a synthetic resin. Therefore, a resin molded product obtained using the resin composition has various advantages such as an increase in tensile strength, an increase in elastic modulus, an improvement in heat resistance, an improvement in flame retardancy, and an improvement in gas barrier properties. is there.
本発明の樹脂組成物は、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩を１〜２０重量％含有してなるものである。 The resin composition of the present invention comprises 1 to 20% by weight of layered silicate in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more.
本発明で用いるエチレン−酢酸ビニル共重合体は、酢酸ビニル濃度が１０重量％以上である。酢酸ビニル濃度が１０重量％未満であると、後述する層状ケイ酸塩の分散性が悪化する。酢酸ビニル濃度の上限は特に指定されないが、３０重量％程度である。
このようなエチレン−酢酸ビニル共重合体は、他の樹脂を比較して極性が高いため、層状ケイ酸塩の層剥離に影響を与えやすいものと推察する。
The ethylene-vinyl acetate copolymer used in the present invention has a vinyl acetate concentration of 10% by weight or more. When the vinyl acetate concentration is less than 10% by weight, the dispersibility of the layered silicate described later deteriorates. The upper limit of the vinyl acetate concentration is not particularly specified, but is about 30% by weight.
Since such an ethylene-vinyl acetate copolymer has a higher polarity than other resins, it is presumed that it easily affects the delamination of the layered silicate.
本発明の樹脂組成物に用いる層状ケイ酸塩としては、ベントナイト、モンモリロナイト、バイデライト、サポナイト、ヘクトライト、バーミュキュライト、白雲母、金雲母、フッ素四珪素雲母、カオリナイト、セピオライト、カネマイト、マガディアイト、トバモライト、フライポンタイト等が挙げられ、これらは天然品であっても合成品であってもよい。本発明においては上記層状ケイ酸塩を単独で用いることも、２種以上を組み合わせて用いることもできる。
本発明の層状ケイ酸塩の粒の大きさは好ましくは０．５〜６ｍｍ、より好ましくは０．８〜５ｍｍ、特に好ましくは１〜３ｍｍである。また、その形状は特に制限はなく、破砕粒、転動造粒、押し出し造粒およびフレーク状粒の何れでもよいが、好ましくはフレーク状粒であり、さらに好ましくはフレーク状粒の形状の厚さが０．１〜２．０ｍｍであり、かつ平均アスペクト比が３〜５０、より好ましくは厚さが０．４〜１．０ｍｍであり、かつ、平均アスペクト比が５〜２０の小片である（ここでアスペクト比とは、平板状粒子の主平面の投影面積の円相当径の直径を粒子の厚みで除したものの平均値をいう）。
Examples of the layered silicate used in the resin composition of the present invention include bentonite, montmorillonite, beidellite, saponite, hectorite, vermiculite, muscovite, phlogopite, fluorotetrasilicon mica, kaolinite, sepiolite, kanemite, magadia And the like. These may be natural products or synthetic products. In the present invention, the layered silicate can be used alone or in combination of two or more.
The grain size of the layered silicate of the present invention is preferably 0.5 to 6 mm, more preferably 0.8 to 5 mm, and particularly preferably 1 to 3 mm. The shape is not particularly limited, and may be any of crushed particles, rolling granulation, extrusion granulation, and flaky particles, preferably flaky particles, and more preferably the thickness of the flaky particle shape. Is a small piece having an average aspect ratio of 3 to 50, more preferably a thickness of 0.4 to 1.0 mm, and an average aspect ratio of 5 to 20 (0.1 to 2.0 mm) Here, the aspect ratio means an average value obtained by dividing the diameter of the equivalent circle diameter of the projected area of the main plane of the tabular grain by the grain thickness).
また、上記層状ケイ酸塩は、層間に有機分子や有機イオンをインターカレーションして、親有機化したものが好ましく用いられる。
このように親有機化された層状ケイ酸塩は、親有機化されていない層状ケイ酸塩と比較して層剥離が起こりやすく、マトリックス中に分散しやすい傾向にある。
In addition, the layered silicate is preferably made of an organic molecule or an organic ion intercalated between layers to make it hydrophilic.
The layered silicate that has been made organophilic in this way tends to cause delamination and tends to be dispersed in the matrix as compared with the layered silicate that has not been made organophilic.
上記のような層状ケイ酸塩は一般的に５Å以上の層間隙を有しているが、層状ケイ酸塩自体が親水性であることから、合成樹脂中に添加した場合、両者の界面自由エネルギーの差が大きく、通常は層剥離しにくくそのまま混合すると分散性が悪い。これは、親有機化された層状ケイ酸塩であっても同様である。しかしながら、合成樹脂として、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体を用いた場合には、層状ケイ酸塩の層剥離が良好で、エチレン−酢酸ビニル共重合体中に均一に分散したナノコンポジットの形成が可能となる。 The layered silicate as described above generally has a layer gap of 5 mm or more. However, since the layered silicate itself is hydrophilic, when added to a synthetic resin, the free energy of the interface between the two The difference is large, and usually the layer is difficult to peel off, and when mixed as it is, the dispersibility is poor. The same applies to layered silicates that have been made organophilic. However, when an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more is used as a synthetic resin, the layered silicate has good layer peeling, and the ethylene-vinyl acetate copolymer contains Uniformly dispersed nanocomposites can be formed.
エチレン−酢酸ビニル共重合体中に含有される層状ケイ酸塩は、１〜２０重量％である。１重量％未満であると、層状ケイ酸塩を添加しても樹脂物性の変化が見られくい。また、２０重量％を超えると、層状ケイ酸塩の層剥離が起こりにくくなり、エチレン−酢酸ビニル共重合体中に均一分散しなくなる。 The layered silicate contained in the ethylene-vinyl acetate copolymer is 1 to 20% by weight. When the content is less than 1% by weight, the physical properties of the resin are hardly changed even when layered silicate is added. On the other hand, when it exceeds 20% by weight, the layered silicate is hardly peeled off and is not uniformly dispersed in the ethylene-vinyl acetate copolymer.
本発明の樹脂組成物を用いて得られる樹脂成形品は、層状ケイ酸塩が、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に予め均一分散されていれば、当該酢酸ビニル濃度が１０重量％以上である酢酸ビニル共重合体のみをマトリックスとしなくてもよい。すなわち、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体中に層状ケイ酸塩を均一分散させたマスターバッチと、他の合成樹脂とから樹脂成形品を構成してもよい。 The resin molded product obtained using the resin composition of the present invention is such that the layered silicate is uniformly dispersed in advance in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more. Only the vinyl acetate copolymer having a vinyl concentration of 10% by weight or more may not be used as the matrix. That is, a resin molded product may be composed of a master batch in which a layered silicate is uniformly dispersed in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more and another synthetic resin.
本発明で使用可能な合成樹脂としては、特に限定はないが熱可塑性樹脂、例えばポリエチレン、エチレン系共重合体、ポリプロピレン等のポリオレフィン、ポリ塩化ビニル、ポリアミド、ポリエステル等が挙げられる。 The synthetic resin that can be used in the present invention is not particularly limited, and examples thereof include thermoplastic resins such as polyethylene, ethylene copolymers, polyolefins such as polypropylene, polyvinyl chloride, polyamide, and polyester.
本発明の樹脂成形品は、単層であってもよいし、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩が含有されてなる層、あるいは他の合成樹脂と、予め酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩が含有されてなる樹脂組成物とからなる層を一層以上含む多層構成であってもよい。 The resin molded product of the present invention may be a single layer, a layer in which a layered silicate is contained in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more, or other synthesis A multilayer structure including one or more layers of a resin and a resin composition in which a layered silicate is previously contained in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more may be used.
本発明の樹脂成形品には、必要に応じて更に他の成分を含有していてもよい。例え紫外線吸収剤、光安定剤、顔料等の各種添加剤が使用可能である。 The resin molded product of the present invention may further contain other components as necessary. Various additives such as ultraviolet absorbers, light stabilizers, and pigments can be used.
本発明の樹脂成形品を成形する方法は特に限定されるものではなく、カレンダー成形、インフレーション成形、押出成形、射出成形など、慣用の方法で成形される。 The method for molding the resin molded product of the present invention is not particularly limited, and the resin molded product is molded by a conventional method such as calendar molding, inflation molding, extrusion molding, injection molding or the like.
以下、実施例を挙げて本発明を具体的に説明するが、本発明はこれら実施例により限定されるものではない。 EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated concretely, this invention is not limited by these Examples.
＜実施例１〜６、比較例１〜３＞
層状ケイ酸塩と合成樹脂の混合物を二軸押出機で混練して、樹脂組成物を作製した。
<Examples 1-6, Comparative Examples 1-3>
A mixture of layered silicate and synthetic resin was kneaded with a twin screw extruder to prepare a resin composition.
表中；
・樹脂１
エチレン−酢酸ビニル共重合体 酢酸ビニル含有量６重量％
・樹脂２
エチレン−酢酸ビニル共重合体 酢酸ビニル含有量１８重量％
・樹脂３
エチレン−酢酸ビニル共重合体 酢酸ビニル含有量２５重量％
・樹脂４
低密度ポリエチレン
・層状ケイ酸塩１
親有機化ベントナイト （株）ホージュン社製「エスベンＮＸ」
・層状ケイ酸塩２
親有機化マイカ コープケミカル（株）社製「ソマシフＭＴＥ」
・層状ケイ酸塩３
モンモリロナイト クニミネ工業（株）社製「クニピアＦ」
In the table;
・ Resin 1
Ethylene-vinyl acetate copolymer Vinyl acetate content 6% by weight
・ Resin 2
Ethylene-vinyl acetate copolymer Vinyl acetate content 18% by weight
・ Resin 3
Ethylene-vinyl acetate copolymer Vinyl acetate content 25% by weight
・ Resin 4
Low density polyethylene / Layered silicate 1
Organic Organized Bentonite "Esven NX" manufactured by Hojun Co., Ltd.
・ Layered silicate 2
"Somasif MTE" manufactured by parent organic mica co-op chemical
・ Layered silicate 3
Montmorillonite “Kunipia F” manufactured by Kunimine Industry Co., Ltd.
実施例１〜６、比較例１〜３で得られた各樹脂組成物について、以下の評価を行なった。 The following evaluation was performed about each resin composition obtained in Examples 1-6 and Comparative Examples 1-3.
＜ストランドの外観＞
ベース樹脂だけを混練した後の状態と、樹脂と層状ケイ酸塩との混合物を混練した後の状態を比較し、以下の基準で評価した。
◎・・・ベース樹脂だけの場合と変わらずきれいである
○・・・ベース樹脂だけの場合より若干劣るがきれいである
△・・・ベース樹脂だけの場合と比較して、若干ボソボソしている
×・・・ベース樹脂だけの場合と比較して、目立ってボソボソしている
××・・・混練できなかった
<Appearance of strand>
The state after kneading only the base resin and the state after kneading the mixture of resin and layered silicate were compared and evaluated according to the following criteria.
◎ ・ ・ ・ Beautiful as it is with base resin alone ○ ・ ・ ・ Slightly inferior to that with base resin only, but clean △ ・ ・ ・ Slightly squeezed compared to base resin alone × ・ ・ ・ Compared to the base resin alone.
次に、上記実施例１〜６、比較例１〜２で得られた樹脂組成物を単独で、または他の樹脂と混合し、Ｔダイ押出成形で厚み１００μｍのフィルムを作製した。
なお、実施例１で得られた樹脂組成物を樹脂組成物１、実施例２で得られた樹脂組成物を樹脂組成物２、実施例３で得られた樹脂組成物を樹脂組成物３、実施例４で得られた樹脂組成物を樹脂組成物４、実施例５で得られた樹脂組成物を樹脂組成物５、実施例６で得られた樹脂組成物を樹脂組成物６、比較例１で得られた樹脂組成物を樹脂組成物７、比較例２で得られた樹脂組成物を樹脂組成物８とする。
Next, the resin compositions obtained in Examples 1 to 6 and Comparative Examples 1 and 2 were used alone or mixed with other resins, and films having a thickness of 100 μm were produced by T-die extrusion.
The resin composition obtained in Example 1 is the resin composition 1, the resin composition obtained in Example 2 is the resin composition 2, the resin composition obtained in Example 3 is the resin composition 3, The resin composition obtained in Example 4 is the resin composition 4, the resin composition obtained in Example 5 is the resin composition 5, the resin composition obtained in Example 6 is the resin composition 6, and the comparative example. The resin composition obtained in 1 is referred to as a resin composition 7, and the resin composition obtained in Comparative Example 2 is referred to as a resin composition 8.
なお、樹脂１、３、４は表１に記載の樹脂と同一である。
Resins 1, 3, and 4 are the same as those listed in Table 1.
実施例７〜１５、比較例４〜５で得られた各フィルムについて、以下の評価を行った。 The following evaluation was performed about each film obtained in Examples 7-15 and Comparative Examples 4-5.
＜フィルムの外観＞
フィルムの製膜状態について、以下の基準で評価した。
◎・・・異物が見られない
○・・・ニップすると異物が見られない
△・・・ニップしても多少異物が散見される
×・・・ニップしても異物が目立つ
<Appearance of film>
The film formation state of the film was evaluated according to the following criteria.
◎ ・ ・ ・ No foreign matter is seen ○ ・ ・ ・ No foreign matter is seen when nipped △ ・ ・ ・ Foreign matter is somewhat scattered even after nip × ・ ・ ・ Foreign matter is noticeable even when nipped
＜分散性１＞
得られた各フィルムについて、ＴＥＭ（透過型電子顕微鏡）で層状ケイ酸塩の様子を観察し、以下の基準で評価した。
○・・・凝集物がほとんどない
△・・・凝集物がわずかに見られる
×・・・凝集物が目立つ
<Dispersibility 1>
About each obtained film, the mode of layered silicate was observed with TEM (transmission electron microscope), and the following references | standards evaluated.
○ ・ ・ ・ Agglomerates are scarce △ ・ ・ ・ Agglomerates are slightly seen × ・ ・ ・ Agglomerates are noticeable
＜分散性２＞
実施例７および実施例９で得られたフィルムについて、Ｘ線解析により層状ケイ酸塩の底面間隔を測定した。いずれも、層状ケイ酸塩の底面間隔が３．５ｎｍ以上であったため、「○」と評価した。
<Dispersibility 2>
About the film obtained in Example 7 and Example 9, the bottom face distance of the layered silicate was measured by X-ray analysis. In all cases, the gap between the bottom surfaces of the layered silicate was 3.5 nm or more, and thus was evaluated as “◯”.
上記実施例および比較例の結果から、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩を１〜２０重量％含有してなる樹脂組成物は層状ケイ酸塩の分散性が良好であることがわかる。
また、酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩を１〜２０重量％含有してなる樹脂成形品あるいは予め酢酸ビニル濃度が１０重量％以上であるエチレン−酢酸ビニル共重合体に層状ケイ酸塩を１〜２０重量％含有してなる樹脂組成物と他の合成樹脂とからなる樹脂成形品についても、層状ケイ酸塩が均一に分散していることがわかる。
From the results of the above Examples and Comparative Examples, a resin composition comprising 1 to 20% by weight of a layered silicate in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more is a layered silicate. It can be seen that the dispersibility of is good.
Further, a resin molded product comprising 1 to 20% by weight of a layered silicate in an ethylene-vinyl acetate copolymer having a vinyl acetate concentration of 10% by weight or more, or ethylene having a vinyl acetate concentration of 10% by weight or more in advance. -The layered silicate is also uniformly dispersed in a resin molded product comprising a resin composition containing 1 to 20% by weight of a layered silicate in a vinyl acetate copolymer and another synthetic resin. I understand.
Claims (3)
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| JP2014198009A JP2016069441A (en) | 2014-09-29 | 2014-09-29 | Layered silicate-containing resin composition, and resin molded article obtained by using the same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190149315A1 (en) * | 2016-06-30 | 2019-05-16 | Socionext Inc. | Equalizer circuit, reception circuit, and semiconductor integrated circuit |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20190149315A1 (en) * | 2016-06-30 | 2019-05-16 | Socionext Inc. | Equalizer circuit, reception circuit, and semiconductor integrated circuit |
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