JP2828469B2 - Ethylene copolymer composition for crosslinking for heat shrink tubing - Google Patents
Ethylene copolymer composition for crosslinking for heat shrink tubingInfo
- Publication number
- JP2828469B2 JP2828469B2 JP1223206A JP22320689A JP2828469B2 JP 2828469 B2 JP2828469 B2 JP 2828469B2 JP 1223206 A JP1223206 A JP 1223206A JP 22320689 A JP22320689 A JP 22320689A JP 2828469 B2 JP2828469 B2 JP 2828469B2
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- Prior art keywords
- ethylene
- crosslinking
- copolymer
- meth
- copolymer composition
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Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は柔軟性、引張特性、加工性、架橋特性に優
れ、熱収縮チューブに好適な架橋用エチレン共重合体組
成物およびそれを架橋してなる熱収縮チューブ用架橋エ
チレン共重合体組成物に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention is excellent in flexibility, tensile properties, processability, and cross-linking properties, and is suitable for a heat-shrinkable tube. The present invention relates to a crosslinked ethylene copolymer composition for a heat shrinkable tube.
熱収縮チューブ等はその使用に際して可撓性が必要で
あり、それらに用いられる材料に柔軟性が必要とされ
る。また、熱収縮チューブにおいては耐熱性、耐油性の
向上の為に、及び延伸による収縮性能付与の為に、架橋
されるのが一般的である。このように架橋して用いるた
めには、架橋前の押し出し加工が容易であり、架橋効率
が良く、架橋された重合体が耐熱性、耐油性等熱収縮チ
ューブとして優れた物性を持つことが要求される。Heat shrink tubes and the like need to be flexible when used, and the materials used for them need to be flexible. In general, a heat-shrinkable tube is crosslinked to improve heat resistance and oil resistance, and to impart shrinkage performance by stretching. In order to use such a crosslinked product, it is required that extrusion processing before crosslinking is easy, crosslinking efficiency is good, and the crosslinked polymer has excellent physical properties such as heat resistance and oil resistance as a heat shrinkable tube. Is done.
このような柔軟で架橋可能な材料として、エチレン・
α−オレフィン共重合体、エチレン・ビニルエステル共
重合体、エチレン・（メタ）アクリル酸エステル共重合
体等が知られている。しかしながら、いずれも次のよう
な問題点がある。Such flexible and crosslinkable materials include ethylene
There are known α-olefin copolymers, ethylene / vinyl ester copolymers, ethylene / (meth) acrylate copolymers, and the like. However, both have the following problems.
すなわち、エチレン・α−オレフィン共重合体とし
て、直鎖状低密度ポリエチレンでは、用途によっては柔
軟性が不十分である。また、密度が0.87〜0.89g/cm3程
度のエチレン・プロピレン共重合体では強度が不十分で
ある。That is, the linear low-density polyethylene as the ethylene / α-olefin copolymer has insufficient flexibility depending on the use. Further, an ethylene / propylene copolymer having a density of about 0.87 to 0.89 g / cm 3 has insufficient strength.
一方、密度が0.87〜0.89g/cm3程度の低結晶性エチレ
ン・１−ブテン共重合体は柔軟性、電気特性、機械的強
度などに優れており、絶縁被覆材の用途に使用できるこ
とが例えば特開昭62−295937号公報に開示されている。
しかしながら、その耐熱性、耐油性等を改良するため架
橋処理を施す場合に架橋し難いという欠点がある。例え
ば電子線照射架橋を行う場合、エチレン・酢酸ビニル共
重合体、エチレン・アクリル酸エチル共重合体等に比較
して同一照射線量での架橋度が低く、十分な耐熱性、耐
油性が得られない。また、架橋度を高くすると、エチレ
ン・１−ブテン共重合体の特長とするところの引張強度
の低下が著しくなる。On the other hand, a low-crystalline ethylene / 1-butene copolymer having a density of about 0.87 to 0.89 g / cm 3 is excellent in flexibility, electric properties, mechanical strength, and the like, and can be used for an insulating coating material, for example. It is disclosed in JP-A-62-295937.
However, there is a disadvantage that crosslinking is difficult when a crosslinking treatment is performed to improve the heat resistance, oil resistance and the like. For example, when performing electron beam irradiation crosslinking, the degree of crosslinking at the same irradiation dose is lower than that of ethylene / vinyl acetate copolymer, ethylene / ethyl acrylate copolymer, etc., and sufficient heat resistance and oil resistance are obtained. Absent. When the degree of crosslinking is increased, the tensile strength, which is a feature of the ethylene / 1-butene copolymer, is significantly reduced.
また、エチレン・ビニルエステル共重合体として、エ
チレン・酢酸ビニル共重合体が一般的に使用されるが、
エチレン・酢酸ビニル共重合体は熱によって脱酢酸反応
が容易に起こり、耐熱性に限界がある。Further, as the ethylene-vinyl ester copolymer, ethylene-vinyl acetate copolymer is generally used,
Ethylene / vinyl acetate copolymer easily undergoes deacetic acid reaction by heat, and has a limit in heat resistance.
更に、エチレン・（メタ）アクリル酸エステル共重合
体においては、メルトフローレートの小さいものでない
と引張強度が大きなものとならず、加工性に難点が生ず
る。このようなエチレン・（メタ）アクリル酸エステル
共重合体に直鎖状低密度ポリエチレンを配合して電気絶
縁被覆に用いる例が特開昭63−143704号公報に示されて
いるが、用途によっては柔軟性が不足している。また、
エチレン・（メタ）アクリル酸エステル共重合体にエチ
レン共重合ゴムを配合して、絶縁材料に使用する例が特
開昭62−12005号や特開昭62−292846号などの公報に示
されているが、ゴムを配合するため押出加工性に難点が
ある。Furthermore, in the case of ethylene / (meth) acrylate copolymer, unless the melt flow rate is low, the tensile strength does not become high, and there is a problem in workability. Japanese Patent Application Laid-Open No. 63-143704 discloses an example in which a linear low-density polyethylene is blended with such an ethylene / (meth) acrylate copolymer for use in electrical insulation coating. Lack of flexibility. Also,
JP-A-62-12005 and JP-A-62-292846 disclose examples in which an ethylene copolymer rubber is blended with an ethylene / (meth) acrylate copolymer and used as an insulating material. However, there is a problem in extrudability due to the compounding of rubber.
本発明者らは、加工性、柔軟性、引張特性に優れ、ま
た架橋処理をした場合の架橋効率が高く、架橋後の引張
特性に優れ、したがって耐熱性、耐油性等の向上が容易
な素材について種々検討を行った。その結果、特定のエ
チレン含有量と密度を有する低結晶性のエチレン・１−
ブテン共重合体とエチレン・（メタ）アクリル酸エステ
ル共重合体とを一定の割合で混合した以下に示すような
樹脂組成物がこのような諸条件を満足していることを見
出すに至り、本発明に到達した。The present inventors have developed a material which is excellent in processability, flexibility and tensile properties, has a high crosslinking efficiency when subjected to crosslinking treatment, and has excellent tensile properties after crosslinking, and therefore is easily improved in heat resistance, oil resistance and the like. Were examined in various ways. As a result, low crystalline ethylene 1- 1 having a specific ethylene content and density
The following resin composition in which a butene copolymer and an ethylene / (meth) acrylate copolymer were mixed at a certain ratio satisfied the above-mentioned conditions. The invention has been reached.
［課題を解決するための手段］ 本発明はエチレン含有量が84〜93モル％、密度が0.87
〜0.89g/cm3の低結晶性エチレン・１−ブテン共重合体1
0〜90重量部と、（メタ）アクリル酸エステル含有量が
５〜40重量％のエチレン・（メタ）アクリル酸エステル
共重合体10〜90重量部とを混合してなる熱収縮チューブ
用架橋用エチレン共重合体組成物及び上記組成物を架橋
してなる熱収縮チューブ用架橋エチレン共重合体組成物
である。Means for Solving the Problems The present invention has an ethylene content of 84 to 93 mol% and a density of 0.87.
~0.89g / cm 3 of the low crystalline ethylene-1-butene copolymer 1
For crosslinking of heat-shrinkable tubes obtained by mixing 0 to 90 parts by weight with 10 to 90 parts by weight of an ethylene / (meth) acrylate copolymer having a (meth) acrylate content of 5 to 40% by weight. An ethylene copolymer composition and a crosslinked ethylene copolymer composition for a heat-shrinkable tube obtained by crosslinking the above composition.
本発明で使用するエチレン・１−ブテン共重合体は、
エチレン含有量が84〜93モル％、好ましくは85〜90モル
％、密度が0.87〜0.89g/cm3、好ましくは0.88〜0.89g/c
m3の低結晶性の共重合体である。エチレン含有量が上記
範囲より少ないものは非晶性となり、耐熱性、耐油性、
引張強度が劣るので好ましくない。また、エチレン含有
量が上記範囲より多くなると、共重合体の柔軟性が損な
われるので柔軟な組成物を得ることができない。本発明
の組成物においては上記エチレン・１−ブテン共重合体
が非晶性のゴム状ポリマーではなく、低度の結晶性を有
していることに特長があり、このため適度の柔軟性と優
れた耐熱性、加工性を有している。共重合体の結晶化度
は、Ｘ線回折法で測定して通常10〜30％程度、好ましく
は10〜20％程度である。加工性及び引張特性とのバラン
スから、上記共重合体として、メルトフローレート（19
0℃,2160g荷重）が0.1〜30g/10分、とくに１〜10g/10分
のものを用いるのが好ましい。The ethylene / 1-butene copolymer used in the present invention is
Ethylene content of 84 to 93 mol%, preferably 85-90 mol%, a density of 0.87~0.89g / cm 3, preferably 0.88~0.89g / c
a low crystalline copolymer of m 3. If the ethylene content is less than the above range becomes amorphous, heat resistance, oil resistance,
It is not preferable because the tensile strength is inferior. On the other hand, if the ethylene content exceeds the above range, the flexibility of the copolymer is impaired, so that a flexible composition cannot be obtained. The composition of the present invention is characterized in that the ethylene / 1-butene copolymer is not an amorphous rubbery polymer but has a low degree of crystallinity. Has excellent heat resistance and workability. The crystallinity of the copolymer is usually about 10 to 30%, preferably about 10 to 20%, as measured by an X-ray diffraction method. In consideration of the balance between processability and tensile properties, the above copolymer is used as a melt flow rate (19
(0 ° C, 2160 g load) 0.1 to 30 g / 10 min, preferably 1 to 10 g / 10 min.
本発明で使用されるエチレン・（メタ）アクリル酸エ
ステル共重合体は、（メタ）アクリル酸エステル含有量
が５〜40重量％、好ましくは10〜20重量％のものであ
る。ここに（メタ）アクリル酸エステルは、アクリル酸
又はメタクリル酸のエステルであって、例えば、メチ
ル、エチル、ｎ−又はイソプロピル、ｎ−、イソ、sec
−又はtert−ブチル、ｎ−ヘキシル、ｎ−オクチル、２
−エチルヘキシルなどのエステルである。好ましくはア
クリル酸又はメタクリル酸の炭素数１〜４のアルキルエ
ステルである。（メタ）アクリル酸エステル含有量が上
記範囲より少ないものは柔軟性に乏しく、また上記範囲
より多いものは柔軟すぎ、耐熱性等に劣るので好ましく
ない。該共重合体としては、引張特性、耐熱性、加工性
等のバランスを勘案すると、メルトフローレートが0.1
〜50g/10分、とくに0.1〜10g/分のものが好ましい。The ethylene / (meth) acrylate copolymer used in the present invention has a (meth) acrylate content of 5 to 40% by weight, preferably 10 to 20% by weight. Here, the (meth) acrylic acid ester is an ester of acrylic acid or methacrylic acid, for example, methyl, ethyl, n- or isopropyl, n-, iso, sec.
-Or tert-butyl, n-hexyl, n-octyl, 2
Esters such as ethylhexyl. Preferably, it is a C1-C4 alkyl ester of acrylic acid or methacrylic acid. Those having a (meth) acrylic acid ester content less than the above range are poor in flexibility, and those having a (meth) acrylic ester content in excess of the above range are not preferable because they are too soft and have poor heat resistance. Considering the balance of tensile properties, heat resistance, workability, etc., the copolymer has a melt flow rate of 0.1.
5050 g / 10 min, preferably 0.1 to 10 g / min.
低結晶性エチレン・１−ブテン共重合体とエチレン・
（メタ）アクリル酸エステル共重合体の配合割合は、両
者の合計を100重量部とした場合、前者が10〜90重量
部、好ましくは30〜70重量部に対し、後者が10〜90重量
部、好ましくは30〜70重量部である。前者の割合が前記
範囲より少ないと加工性に優れ、架橋後の引張特性が良
好な架橋物が得難い。また前者の割合が前記範囲より多
くなると架橋効率が悪くなり好ましくない。Low crystalline ethylene / 1-butene copolymer and ethylene
The mixing ratio of the (meth) acrylate copolymer is 10 to 90 parts by weight, preferably 30 to 70 parts by weight, and the latter is 10 to 90 parts by weight, when the total of both is 100 parts by weight. , Preferably 30 to 70 parts by weight. If the former ratio is less than the above range, it is difficult to obtain a crosslinked product having excellent workability and excellent tensile properties after crosslinking. On the other hand, if the ratio of the former is more than the above range, the crosslinking efficiency becomes poor, which is not preferable.
本発明においては上記低結晶性エチレン・１−ブテン
共重合体とエチレン・（メタ）アクリル酸エステル共重
合体からなる組成物は、これを更に架橋することによっ
て物性が著しく改良される。架橋された重合体組成物は
熱収縮性チューブとして卓越した物性を示すので、本発
明組成物は特にこれらの用途には架橋重合体組成物とし
て使用するのに適している。In the present invention, the composition comprising the low-crystalline ethylene / 1-butene copolymer and the ethylene / (meth) acrylate copolymer is remarkably improved in physical properties by further crosslinking. The compositions of the present invention are particularly suitable for use as crosslinked polymer compositions for these applications because the crosslinked polymer compositions exhibit excellent physical properties as heat shrinkable tubes.
架橋は有機過酸化物を用いる方法、電子線照射による
方法など任意の方法を採用することができる。本発明の
上記組成物はいずれの方法を用いても効率よく架橋する
ことができる。For the crosslinking, any method such as a method using an organic peroxide or a method using electron beam irradiation can be adopted. The composition of the present invention can be efficiently cross-linked by any method.
有機過酸化物架橋の場合、ジクミルパ−オキサイド、
ジｔ−ブチルパ−オキサイド、ｔ−ブチルクミルパ−オ
キサイド、などの有機過酸化物を用いることができる。In the case of organic peroxide crosslinking, dicumyl peroxide,
Organic peroxides such as di-t-butyl peroxide and t-butyl cumyl peroxide can be used.
また架橋に際し、トリアリルシアヌレートなどの架橋
助剤を使用することができる。In crosslinking, a crosslinking aid such as triallyl cyanurate can be used.
また架橋の前に上記組成物中に任意の添加剤、例えば
ポリブテン−１のような加工助剤、酸化防止剤、無機充
填剤、顔料、染料、紫外線吸収剤、耐候安定剤、滑剤な
どを配合しておいてもよい。Before crosslinking, optional additives such as processing aids such as polybutene-1, antioxidants, inorganic fillers, pigments, dyes, ultraviolet absorbers, weather stabilizers, lubricants and the like are mixed in the composition before crosslinking. You may keep it.
本発明のエチレン共重合体組成物は、架橋前の押出加
工性に優れ、高い架橋効率で架橋することができ、得ら
れた架橋共重合体組成物は耐熱性、耐油性、柔軟性に優
れているので、熱収縮チューブ用の材料として好適であ
る。The ethylene copolymer composition of the present invention has excellent extrudability before crosslinking and can be crosslinked with high crosslinking efficiency, and the obtained crosslinked copolymer composition has excellent heat resistance, oil resistance and flexibility. Therefore, it is suitable as a material for a heat-shrinkable tube.
以下、実施例及び比較例により本発明を詳細に説明す
る。Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples.
実施例１〜３、比較例１〜２ 下記に示すエチレン・１−ブテン共重合体（EB）とエ
チレン・アクリル酸エステル共重合体（EEA）とを第１
表に示す配合割合に従って、一軸押出機にてメルトブレ
ンドにより混合物とした。Examples 1 to 3 and Comparative Examples 1 and 2 An ethylene / 1-butene copolymer (EB) and an ethylene / acrylate copolymer (EEA) shown below were first used.
According to the compounding ratio shown in the table, a mixture was obtained by melt blending using a single screw extruder.
EEA:エチレン・アクリル酸エチル共重合体 （アクリル酸エチル含量15重量％） MFR 0.5g/10分、 EB :エチレ・ブテン−１共重合体 （エチレン85モル％） MFR 3.6g/10分 結晶化度 10％ 密度0.88g/cm3 得られた混合物をプレス成形により厚さ0.6mmのシー
トとし、その架橋前の物性を測定した後、日新ハイボル
テージ社製電子線照射装置EPS−750により所定の照射線
量の電子線を照射して架橋し、架橋後の物性を評価し
た。各物性の評価は次の方法に従った。EEA: Ethylene / ethyl acrylate copolymer (ethyl acrylate content 15% by weight) MFR 0.5 g / 10 min, EB: Ethyle / butene-1 copolymer (ethylene 85 mol%) MFR 3.6 g / 10 min Crystallization 10% Density 0.88 g / cm 3 The obtained mixture was formed into a sheet having a thickness of 0.6 mm by press molding, and its physical properties before cross-linking were measured. Then, the sheet was specified using an electron beam irradiator EPS-750 manufactured by Nissin High Voltage. Was irradiated with an electron beam at an irradiation dose of, and the physical properties after crosslinking were evaluated. Each physical property was evaluated according to the following methods.
（１）メルトフローレート（MFR） JISK6760に準拠し、温度190℃、荷重2160gにて測定し
た。(1) Melt flow rate (MFR) Measured at a temperature of 190 ° C. and a load of 2160 g in accordance with JIS K6760.
（２）引張特性 架橋前後いずれも厚さ0.6mmのシートを用い、JISK630
1の３号試験片としてJISK6760に準拠して測定した。(2) Tensile properties JISK630
Measured according to JISK6760 as No. 3 test piece.
（３）ゲル分率 架橋物1gを100mlのキシレン中に110℃、24時間浸漬し
たのち、不溶解分を回収、乾燥後秤量し、浸漬前重量に
対する比率を算出した。(3) Gel fraction After 1 g of the crosslinked product was immersed in 100 ml of xylene at 110 ° C for 24 hours, the insoluble matter was recovered, dried and weighed, and the ratio to the weight before immersion was calculated.
（４）ねじり剛性率 厚さ3mmのシートを用い、JIS K6730に準拠して測定し
た。(4) Torsional rigidity A 3 mm-thick sheet was measured in accordance with JIS K6730.
上記の試験による架橋前および架橋後の共重合体組成
物の物性を第１表に示した。Table 1 shows the physical properties of the copolymer composition before and after crosslinking according to the above test.
フロントページの続き (56)参考文献 特開 昭63−143704（ＪＰ，Ａ) 特開 昭64−69650（ＪＰ，Ａ) 特開 昭63−205340（ＪＰ，Ａ) 特開 平２−258851（ＪＰ，Ａ) 特開 平２−113045（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) C08L 23/00 - 23/36Continuation of the front page (56) References JP-A-63-143704 (JP, A) JP-A-64-69650 (JP, A) JP-A-63-205340 (JP, A) JP-A-2-258851 (JP , A) JP-A-2-113045 (JP, A) (58) Fields investigated (Int. Cl. 6 , DB name) C08L 23/00-23/36
Claims (2)
87〜0.89g/cm3の低結晶性エチレン・１−ブテン共重合
体10〜90重量部と、（メタ）アクリル酸エステル含有量
が５〜40重量％のエチレン・（メタ）アクリル酸エステ
ル共重合体10〜90重量部とを混合してなる熱収縮チュー
ブ用架橋用エチレン共重合体組成物。(1) an ethylene content of 84 to 93 mol% and a density of 0.
10 to 90 parts by weight of a low crystalline ethylene / 1-butene copolymer of 87 to 0.89 g / cm 3 and ethylene / (meth) acrylate having a (meth) acrylate content of 5 to 40% by weight An ethylene copolymer composition for crosslinking for a heat-shrinkable tube, which is obtained by mixing 10 to 90 parts by weight of a polymer.
架橋してなる熱収縮チューブ用架橋エチレン共重合体組
成物。2. A crosslinked ethylene copolymer composition for a heat-shrinkable tube obtained by crosslinking the ethylene copolymer composition according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1223206A JP2828469B2 (en) | 1989-08-31 | 1989-08-31 | Ethylene copolymer composition for crosslinking for heat shrink tubing |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1223206A JP2828469B2 (en) | 1989-08-31 | 1989-08-31 | Ethylene copolymer composition for crosslinking for heat shrink tubing |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0386742A JPH0386742A (en) | 1991-04-11 |
| JP2828469B2 true JP2828469B2 (en) | 1998-11-25 |
Family
ID=16794457
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1223206A Expired - Fee Related JP2828469B2 (en) | 1989-08-31 | 1989-08-31 | Ethylene copolymer composition for crosslinking for heat shrink tubing |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2828469B2 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4746197B2 (en) * | 2001-04-03 | 2011-08-10 | 住友電気工業株式会社 | Resin composition containing thermoplastic polyurethane and heat-shrinkable tube using the same |
| JPWO2017038374A1 (en) * | 2015-08-28 | 2018-02-15 | 三井化学東セロ株式会社 | Electron beam crosslinkable ethylene resin composition, electron beam cross-linked product, method for producing electron beam cross-linked product, and laminate |
| US10898616B1 (en) | 2017-07-11 | 2021-01-26 | Teleflex Medical Incorporated | Peelable heat-shrink tubing |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63205340A (en) * | 1987-02-19 | 1988-08-24 | Fujikura Ltd | Semiconductive mixture |
| JPH07103276B2 (en) * | 1987-09-11 | 1995-11-08 | 日本石油化学株式会社 | Ethylene-based thermoplastic resin composition |
| JP2740204B2 (en) * | 1988-10-20 | 1998-04-15 | 三井化学株式会社 | Thermoplastic elastomer composition |
| JPH02258851A (en) * | 1989-03-31 | 1990-10-19 | Fujikura Ltd | Electrical insulating resin composition |
-
1989
- 1989-08-31 JP JP1223206A patent/JP2828469B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0386742A (en) | 1991-04-11 |
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