JPH08208913A - Ethylene/alpha-olefin copolymer rubber composition - Google Patents
Ethylene/alpha-olefin copolymer rubber compositionInfo
- Publication number
- JPH08208913A JPH08208913A JP3935195A JP3935195A JPH08208913A JP H08208913 A JPH08208913 A JP H08208913A JP 3935195 A JP3935195 A JP 3935195A JP 3935195 A JP3935195 A JP 3935195A JP H08208913 A JPH08208913 A JP H08208913A
- Authority
- JP
- Japan
- Prior art keywords
- ethylene
- copolymer rubber
- olefin copolymer
- rubber
- pts
- Prior art date
- 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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Links
Landscapes
- Sealing Material Composition (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、エチレン-α-オレフィ
ン系共重合ゴム組成物に関する。更に詳しくは、耐ガス
透過性の要求される摺動用シール材の成形材料などとし
て好適に用いられるエチレン-α-オレフィン系共重合ゴ
ム組成物に関する。TECHNICAL FIELD The present invention relates to an ethylene-α-olefin copolymer rubber composition. More specifically, it relates to an ethylene-α-olefin-based copolymer rubber composition that is preferably used as a molding material for a sealing material for sliding that requires gas permeation resistance.
【０００２】[0002]
【従来の技術】エチレン-プロピレン共重合ゴムによっ
て代表されるエチレン-α-オレフィン共重合ゴムあるい
はこれにエチリデンノルボルネン、1,4-ヘキサジエン、
ジシクロペンタジエン等のジエンを更に共重合させたエ
チレン-α-オレフィン-ジエン共重合ゴムであるエチレ
ン-α-オレフィン系共重合ゴムは、耐熱性、耐油性、耐
摩耗性、耐水性などにすぐれており、特にそれらのパー
オキサイド架橋物は圧縮永久歪が小さいため、Oリン
グ、ガスケット等の固定用シールを始め、摺動用シール
材としても広く使用されている。2. Description of the Related Art Ethylene-α-olefin copolymer rubber represented by ethylene-propylene copolymer rubber or ethylidene norbornene, 1,4-hexadiene,
The ethylene-α-olefin copolymer rubber, which is an ethylene-α-olefin-diene copolymer rubber obtained by further copolymerizing a diene such as dicyclopentadiene, has excellent heat resistance, oil resistance, abrasion resistance, water resistance, etc. In particular, since these peroxide cross-linked products have a small compression set, they are widely used as sealing materials for fixing such as O-rings and gaskets as well as sliding sealing materials.
【０００３】特に、エチレン-α-オレフィン系共重合ゴ
ムは、水やグリコール系などの極性の高いシール対象液
に対しての耐性にすぐれているため、自動車用ラジエー
ター、ウォーターポンプ等の水/LLC(ロング・ライフ・
クーラント)のシール、更にはブレーキ関係のシールな
どの成形材料としても多く用いられている。しかしなが
ら、これから成形されたシール材は耐ガス透過性の点で
乏しく、例えばピストン型アキュームレーター等の摺動
部シールに用いた場合、ガスの浸透漏れによる性能の低
下がしばしば問題となっている。In particular, ethylene-α-olefin copolymer rubbers have excellent resistance to liquids having high polarity such as water and glycols, and therefore, water / LLC for automobile radiators, water pumps, etc. (long life·
It is often used as a molding material for seals for coolants and for brakes. However, the sealing material formed from this is poor in gas permeation resistance, and when it is used, for example, in a sliding part seal of a piston type accumulator or the like, deterioration of performance due to gas permeation leakage often becomes a problem.
【０００４】一般的に、極性の高いゴム材料は耐ガス透
過性にすぐれているが、極性の高いシール対象液に対し
ての耐性には乏しく、エチレン-α-オレフィン系共重合
ゴムはその逆の性質を有している。これらの事実は、耐
ガス透過性と極性の高いシール対象液に対する耐性とを
同時に兼ね備えることは困難であることを意味する。Generally, a highly polar rubber material is excellent in gas permeation resistance, but is poor in resistance to a highly polar liquid to be sealed, and an ethylene-α-olefin copolymer rubber is the opposite. It has the property of These facts mean that it is difficult to have both gas permeation resistance and resistance to a highly polar liquid to be sealed at the same time.
【０００５】もっとも、これらの性質を同時に兼備した
ゴム材料も存在し、それの代表的なものはブチルゴムで
あるが、このものは耐摩耗性に乏しく、粘着性をも有す
るため、摺動用シール材料としては不適当である。However, there is also a rubber material having both of these properties at the same time, and a typical one thereof is butyl rubber, but this material has poor abrasion resistance and also has adhesiveness, so that it is a sliding sealing material. Is unsuitable as
【０００６】[0006]
【発明が解決しようとする課題】本発明の目的は、摺動
用シール材の成形材料などとして好適に用いられるエチ
レン-α-オレフィン系共重合ゴム組成物であって、この
共重合ゴムが本来有する好ましい性質、特に極性の高い
シール対象液に対する耐性を損なうことなく、耐ガス透
過性を改善せしめたものを提供することにある。An object of the present invention is to provide an ethylene-α-olefin copolymer rubber composition which is preferably used as a molding material for a sealing material for sliding, which copolymer rubber originally has. It is an object of the present invention to provide a gas having improved gas permeation resistance without impairing preferable properties, particularly resistance to a highly polar liquid to be sealed.
【０００７】[0007]
【課題を解決するための手段】かかる本発明の目的は、
エチレン-α-オレフィン系共重合ゴム、薄片状充填剤お
よび有機過酸化物を含有するエチレン-α-オレフィン系
共重合ゴム組成物によって達成される。SUMMARY OF THE INVENTION The object of the present invention is as follows.
It is achieved by an ethylene-α-olefin copolymer rubber, an ethylene-α-olefin copolymer rubber composition containing a flaky filler and an organic peroxide.
【０００８】前記の如きエチレン-α-オレフィン系共重
合ゴムに添加される薄片状充填剤としては、アスペクト
比(フレーク径/フレーク厚さ)が約10以上、好ましくは
約50以上の薄片状の結晶構造を有するけい酸マグネシウ
ム系充填剤、けい酸アルミニウム系充填剤(天然マイカ)
等が、エチレン-α-オレフィン系共重合ゴム100重量部
当り10〜150重量部、好ましくは30〜100重量部の割合で
用いられる。アスペクト比約10〜50程度の充填剤をこれ
以下の割合で用いると、耐ガス透過性の改善が見込め
ず、一方これ以上の割合で添加すると、加硫物性が低下
するようになる。The flaky filler added to the ethylene-α-olefin copolymer rubber as described above is a flaky filler having an aspect ratio (flake diameter / flake thickness) of about 10 or more, preferably about 50 or more. Magnesium silicate filler having crystal structure, aluminum silicate filler (natural mica)
And the like are used in a proportion of 10 to 150 parts by weight, preferably 30 to 100 parts by weight, per 100 parts by weight of the ethylene-α-olefin copolymer rubber. When a filler having an aspect ratio of about 10 to 50 is used in a ratio less than this, improvement in gas permeation resistance cannot be expected, while when added in a ratio higher than this, vulcanization physical properties are deteriorated.
【０００９】架橋剤としては、イオウ、有機過酸化物の
いずれをも用い得るものの、圧縮永久歪特性の良好な有
機過酸化物が、一般にエチレン-α-オレフィン系共重合
ゴム100重量部当り約0.5〜10重量部、好ましくは約2〜4
重量部の割合で用いられる。有機過酸化物としては、一
般的に用いられているものをそのまま用いることができ
る。As the cross-linking agent, both sulfur and organic peroxide can be used, but an organic peroxide having a good compression set characteristic is generally used in an amount of about 100 parts by weight of ethylene-α-olefin copolymer rubber. 0.5-10 parts by weight, preferably about 2-4
Used in parts by weight. As the organic peroxide, those generally used can be used as they are.
【００１０】以上の各成分を必須成分とする組成物中に
は、補強剤、可塑剤、老化防止剤等が必要に応じて適宜
配合される。補強剤としては、硬度の調整作用をも含
め、カーボンブラック等が用いられる。パラフィン系プ
ロセスオイルが一般に用いられる軟化剤については、こ
れがシール対象液によって抽出されてしまい、収縮によ
るシール性の悪化をひき起こす可能性があり、また耐ガ
ス透過性をも低下させるため、無添加が好ましい。A reinforcing agent, a plasticizer, an antiaging agent and the like are appropriately blended in the composition containing the above-mentioned respective components as essential components. As the reinforcing agent, carbon black or the like is used, including the effect of adjusting hardness. Paraffin-based process oil is generally used as a softening agent, and it may be extracted by the liquid to be sealed, which may cause deterioration of the sealing property due to shrinkage, and also reduces gas permeation resistance. Is preferred.
【００１１】組成物の調製は、オープンロール等の開放
式混練機、ニーダ、インターミキサ等の密閉式混練機な
どを用いて行われる。開放式混練機が用いられる場合に
は、エチレン-α-オレフィン系共重合ゴムをオープンロ
ールに巻き付かせ、素練りした後、架橋剤以外の各配合
成分を少量宛添加し、最後に架橋剤を添加することが行
われる。この間、常時約10Ｌ/分程度の冷却水を流し
て、混練時の温度を約50〜70℃程度に保つことが好まし
い。また、密閉式混練機を用いる場合には、架橋剤以外
の各配合成分を一括して密閉式混練機中に投入して混練
を行い、数分後に排出させてから、オープンロールを用
いて架橋剤の添加が行われる。この間、やはり十分な冷
却水を流し、密閉式混練中は約120℃以下に、またオー
プンロールでの架橋剤添加は約70℃以下に温度を保つこ
とが好ましい。The composition is prepared by using an open type kneader such as an open roll or a closed type kneader such as a kneader or an intermixer. When an open-type kneader is used, ethylene-α-olefin copolymer rubber is wrapped around an open roll, masticated, and then each compounding component other than the crosslinking agent is added in small amounts, and finally the crosslinking agent is added. Is added. During this period, it is preferable to constantly flow about 10 L / min of cooling water to maintain the temperature during kneading at about 50 to 70 ° C. Further, when using a closed kneader, each compounding component other than the cross-linking agent is put into the closed kneader all at once to perform kneading, and after a few minutes, the mixture is discharged and then crosslinked using an open roll. The agent is added. During this time, it is preferable to keep sufficient cooling water to keep the temperature at about 120 ° C. or less during the closed kneading and at about 70 ° C. or less for the addition of the cross-linking agent by the open roll.
【００１２】このようにして調製された組成物は、一般
に約160〜170℃、約15〜20分間の加硫条件下で加硫成形
される。The composition thus prepared is generally vulcanized and molded under vulcanizing conditions of about 160 to 170 ° C. for about 15 to 20 minutes.
【００１３】[0013]
【発明の効果】エチレン-α-オレフィン系共重合ゴム
は、摺動用シール材の成形材料などとして広く用いられ
ており、その充填剤として薄片状のものを用いることに
より、その有機過酸化物架橋物が本来有する好ましい性
質、特に極性の高いシール対象液に対する耐性を損なう
ことなく、耐ガス透過性を改善させることができる。EFFECT OF THE INVENTION Ethylene-α-olefin copolymer rubber is widely used as a molding material for a sliding seal material, and by using a flaky filler as a filler, its organic peroxide cross-linking can be achieved. The gas permeation resistance can be improved without impairing the desirable properties inherent to the object, particularly the resistance to the highly polar liquid to be sealed.
【００１４】[0014]
【実施例】次に、実施例について本発明を説明する。Next, the present invention will be described by way of examples.
【００１５】実施例 エチレン-プロピレン-エチリデンノルボルネン共重合ゴ
ム(日本合成ゴム製品JSR EP33)100部(重量、以下同じ)
に、下記配合剤を所定部数添加し、12インチオープンロ
ールを用いて前記の如き混練方法で混練した後、混練物
を170℃、15分間の条件下で架橋して、厚さ2mmの加硫シ
ートを作製した。 配合剤(部) No.1 No.2 No.3 No.4 No.5 No.6 No.7 天然マイカ(アスペクト比90) 50 80 120 151 〃 ( 〃 30) 9 80 亜鉛華3号(堺化学製品) 5 5 5 5 5 5 5 ステアリン酸 0.5 0.5 0.5 0.5 0.5 0.5 0.5 老化防止剤RD 0.5 0.5 0.5 0.5 0.5 0.5 0.5 〃 MB 2 2 2 2 2 2 2 ジクミルパーオキサイド 3 3 3 3 3 3 3 FEFカーボンブラック 80 80 45 60 45 15 5 注）天然マイカ(アスペクト比90)：プロゴタイプ系、マリエッタ社製品 スゾライト・マイカ40-S 天然マイカ(アスペクト比30)：プロゴタイプ系、マリエッタ社製品 スゾライト・マイカ325-K1 老化防止剤RD：ポリメライズド2,2,4-トリメチル-1,2-ジヒドロ キノリン、精工化学製品 老化防止剤MB：2-メルカプトベンゾイミダゾール、大内新興化学製品 ジクミルパーオキサイド：日本油脂製品パークミルD エステル-エーテル系可塑剤：旭電化製品アデカサイザーRS107Example 100 parts of ethylene-propylene-ethylidene norbornene copolymer rubber (Japan Synthetic Rubber Product JSR EP33) (weight, the same below)
In addition, after adding a predetermined number of the following compounding ingredients and kneading by the kneading method as described above using a 12 inch open roll, the kneaded product is crosslinked at 170 ° C for 15 minutes, and vulcanized to a thickness of 2 mm. A sheet was prepared. Compounding agent (part) No.1 No.2 No.3 No.4 No.5 No.6 No.7 Natural mica (aspect ratio 90) 50 80 120 151 〃 (〃 30) 9 80 Zinhua No. 3 (Sakai Chemical products) 5 5 5 5 5 5 5 5 Stearic acid 0.5 0.5 0.5 0.5 0.5 0.5 0.5 Anti-aging agent RD 0.5 0.5 0.5 0.5 0.5 0.5 0.5 〃 MB 2 2 2 2 2 2 2 Dicumyl peroxide 3 3 3 3 3 3 3 3 FEF carbon black 80 80 45 60 45 15 5 Note) Natural mica (aspect ratio 90): Progo type, Marietta product Szolite Mica 40-S Natural mica (aspect ratio 30): Progo type, Marietta product Szolite Mica 325-K1 Anti-aging agent RD: Polymerized 2,2,4-trimethyl-1,2-dihydroquinoline, a precision chemical product Anti-aging agent MB: 2-mercaptobenzimidazole, Ouchi emerging chemical product Dicumyl peroxide: Japan Oil and fat products Perkmill D Ester-ether plasticizer: Asahi Denka Adeka Sizer RS107
【００１６】得られた加硫シートについて、次の各項目
の測定を行った。 加硫物性：JIS K-6301準拠 圧縮永久歪：120℃、70時間 耐熱老化試験：120℃、70時間後の加硫物性変化 耐液性試験：120℃のブレーキ液DOT 3中に70時間浸漬し
た後の物性変化 N2ガス透過試験：東洋精機製作所製ガス透過率測定装置
を用い、25℃で測定 摩耗試験：砥石H-18、荷重1kg、回転数60rpm×1000回の
条件下でのテーバー摩耗量The following items were measured on the obtained vulcanized sheet. Vulcanization physical properties: JIS K-6301 compliant Compression set: 120 ° C, 70 hours Heat aging test: 120 ° C, change in vulcanization properties after 70 hours Liquid resistance test: Immersed in 120 ° C brake fluid DOT 3 for 70 hours Change in physical properties after being subjected to N 2 gas permeation test: Measured at 25 ° C using a gas permeability measuring device manufactured by Toyo Seiki Seisakusho Co., Ltd. Wear test: Grindstone H-18, load 1 kg, rotation speed 60 rpm × 1000 times Taber Amount of wear
【００１７】測定結果は、次の表に示される。この結果
から、エチレン-プロピレン-エチリデンノルボルネン共
重合ゴム100重量部当り10〜150重量部の薄片状天然マイ
カを配合した有機過酸化物架橋物は、それが本来有する
耐液性を損なうことなく、耐ガス透過性を大幅に改善し
得ることが分かる。 表 測定項目 No.1 No.2 No.3 No.4 No.5 No.6 No.7 No.8 加硫物性 硬さ (JIS A) 80 82 83 82 83 82 89 80 引張強さ (MPa) 21 22 20 18 17 18 13 15 伸び (%) 180 170 150 150 140 100 80 200 圧縮永久歪 (%) 10 12 22 20 25 30 37 12 耐熱老化試験 硬さ変化(ポイント) +1 +1 +1 +1 +1 +1 +1 +3 引張強さ変化率 (%) +2 +6 +4 +12 +8 +11 +8 +8 伸び変化率 (%) -4 -18 -11 -11 -19 -20 -30 -11 耐液性試験 硬さ変化(ポイント) -3 -3 -3 -3 -3 -2 -3 -5 引張強さ変化率 (%) -5 -6 -2 -6 -1 -4 -1 -6 伸び変化率 (%) -4 -11 -7 -7 -6 -5 -6 +7 体積変化率 (%) +3.1 +2.9 +2.9 +3.1 +2.9 +2.8 +2.6 +4.5 N2ガス透過係数 230 225 98 95 85 72 52 10 (cc・mm/cm2・atm・24hrs) テーバー摩耗量 (mg) 150 155 115 130 120 115 120 460 なお、併記されたNo.8は、 ブチルゴム(エクソン製品Butyl 365) 100部 亜鉛華3号(堺化学製品) 5部 ステアリン酸 1部 FEFカーボンブラック 85部 臭素化アルキルフェノール・ホルムアルデヒド樹脂 10部 (住友化学製品タッキロール250III) の混練物から得られた加硫シートについての測定値であ
り、摩耗試験では粘り付きがみられた。The measurement results are shown in the following table. From this result, ethylene-propylene-ethylidene norbornene copolymer rubber 100 to 100 parts by weight of the organic peroxide crosslinked product containing 10 to 150 parts by weight of flaky natural mica, without impairing the liquid resistance that it originally has, It can be seen that the gas permeation resistance can be greatly improved. Table Measurement items No.1 No.2 No.3 No.4 No.5 No.6 No.7 No.8 Vulcanization physical properties Hardness (JIS A) 80 82 83 82 83 82 89 80 Tensile strength (MPa) 21 22 20 18 17 18 13 15 Elongation (%) 180 170 150 150 140 100 80 200 Compression set (%) 10 12 22 20 25 30 37 12 Heat aging test Hardness change (points) +1 +1 +1 + 1 +1 +1 +1 +3 Tensile strength change rate (%) +2 +6 +4 +12 +8 +11 +8 +8 Elongation change rate (%) -4 -18 -11 -11 -19- 20 -30 -11 Liquid resistance test Hardness change (point) -3 -3 -3 -3 -3 -2 -3 -5 Tensile strength change rate (%) -5 -6 -2 -6 -1- 4 -1 -6 Elongation change rate (%) -4 -11 -7 -7 -6 -5 -6 -6 +7 Volume change rate (%) +3.1 +2.9 +2.9 +3.1 +2.9 +2.8 +2.6 +4.5 N 2 Gas permeation coefficient 230 225 98 95 85 72 52 10 (cc ・ mm / cm 2・ atm ・ 24hrs) Taber wear amount (mg) 150 155 115 130 120 115 120 460 No. 8 written together is butyl rubber ( Exxon products Butyl 365) 100 parts Zinc Hua No. 3 (Sakai Chemicals) 5 parts Stearic acid 1 part FEF carbon black 85 parts Brominated alkylphenol-formua It is a measure of the vulcanized sheet obtained from the kneaded product of the dehydrogenase resin 10 parts (Sumitomo Chemical product Tackirol 250III), was observed with stickiness in wear test.
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【手続補正書】[Procedure amendment]
【提出日】平成７年１０月１９日[Submission date] October 19, 1995
【手続補正１】[Procedure amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１５[Correction target item name] 0015
【補正方法】変更[Correction method] Change
【補正内容】[Correction contents]
【００１５】実施例 エチレン−プロピレン−エチリデンノルボルネン共重合
ゴム（日本合成ゴム製品ＪＳＲ ＥＰ３３）１００部
（重量、以下同じ）に、下記配合剤を所定部数添加し、
１２インチオープンロールを用いて前記の如き混練方法
で混練した後、混練物を１７０℃、１５分間の条件下で
架橋して、厚さ２ｍｍの加硫シートを作製した。 Example To 100 parts (weight, hereinafter the same) of ethylene-propylene-ethylidene norbornene copolymer rubber (Japan Synthetic Rubber Product JSR EP33) was added the prescribed amount of the following compounding agent,
After kneading by a kneading method as described above using a 12-inch open roll, the kneaded product was crosslinked under the conditions of 170 ° C. for 15 minutes to prepare a vulcanized sheet having a thickness of 2 mm.
Claims (2)
薄片状充填剤および有機過酸化物を含有してなるエチレ
ン-α-オレフィン系共重合ゴム組成物。1. An ethylene-α-olefin copolymer rubber,
An ethylene-α-olefin copolymer rubber composition comprising a flaky filler and an organic peroxide.
れる請求項１記載のエチレン-α-オレフィン系共重合ゴ
ム組成物。2. The ethylene-α-olefin copolymer rubber composition according to claim 1, which is used as a molding material for a sliding seal material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3935195A JPH08208913A (en) | 1995-02-03 | 1995-02-03 | Ethylene/alpha-olefin copolymer rubber composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3935195A JPH08208913A (en) | 1995-02-03 | 1995-02-03 | Ethylene/alpha-olefin copolymer rubber composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08208913A true JPH08208913A (en) | 1996-08-13 |
Family
ID=12550664
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3935195A Pending JPH08208913A (en) | 1995-02-03 | 1995-02-03 | Ethylene/alpha-olefin copolymer rubber composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08208913A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002194156A (en) * | 2000-12-26 | 2002-07-10 | Mitsubishi Cable Ind Ltd | Rubber composition for sealant and sealant using it |
| WO2006137420A1 (en) * | 2005-06-24 | 2006-12-28 | Nok Corporation | Epdm composition |
| WO2019058908A1 (en) | 2017-09-21 | 2019-03-28 | Nok株式会社 | Epichlorohydrin rubber composition, crosslinked epichlorohydrin rubber object, and diaphragm and bladder for accumulator |
| WO2022050098A1 (en) * | 2020-09-02 | 2022-03-10 | Nok株式会社 | Ethylene/propylene copolymer rubber composition |
-
1995
- 1995-02-03 JP JP3935195A patent/JPH08208913A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002194156A (en) * | 2000-12-26 | 2002-07-10 | Mitsubishi Cable Ind Ltd | Rubber composition for sealant and sealant using it |
| WO2006137420A1 (en) * | 2005-06-24 | 2006-12-28 | Nok Corporation | Epdm composition |
| WO2019058908A1 (en) | 2017-09-21 | 2019-03-28 | Nok株式会社 | Epichlorohydrin rubber composition, crosslinked epichlorohydrin rubber object, and diaphragm and bladder for accumulator |
| WO2022050098A1 (en) * | 2020-09-02 | 2022-03-10 | Nok株式会社 | Ethylene/propylene copolymer rubber composition |
| JPWO2022050098A1 (en) * | 2020-09-02 | 2022-03-10 | ||
| CN115996979A (en) * | 2020-09-02 | 2023-04-21 | Nok株式会社 | Ethylene-propylene copolymer rubber composition |
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