JP2008179783A5 - - Google Patents
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- JP2008179783A5 JP2008179783A5 JP2007324439A JP2007324439A JP2008179783A5 JP 2008179783 A5 JP2008179783 A5 JP 2008179783A5 JP 2007324439 A JP2007324439 A JP 2007324439A JP 2007324439 A JP2007324439 A JP 2007324439A JP 2008179783 A5 JP2008179783 A5 JP 2008179783A5
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本発明は、ゴム組成物およびその用途に関する。詳しくは、本発明は、燃料電池シール材、ＬＩＭ成形用ガスケット材などの各種ガスケット材、電線コネクター用シール材などの用途に好適に用いることのできるゴム組成物、および該ゴム組成物より得られる燃料電池シール材、ハードディスクドライブトップカバーガスケット、ＬＩＭ成形用ガスケット材、電線コネクター用シール材、並びにそれらを実装した本体に関する。 The present invention relates to a rubber composition and use thereof. Specifically, the present invention provides a fuel cell sealing member, obtained from LIM various gasket materials, such as molding the gasket material, a rubber composition can be suitably used in applications such as for electric wire connector sealing member, and the rubber composition The present invention relates to a fuel cell seal material, a hard disk drive top cover gasket, a LIM molding gasket material, a wire connector seal material, and a main body on which they are mounted.
（式［II］中、Ｒ3は炭素数１〜１０の一価の基で、非置換あるいは置換の飽和炭化水素基または芳香族炭化水素基であり、１分子内で同種でも異種でもよく、ａは０〜２０の整数であり、ｂは０〜２０の整数であり、Ｒ4は炭素数１〜３０の二価の有機基または酸素原子である。）
また本発明のゴム組成物が架橋剤［Ｄ］を含む場合、架橋剤［Ｄ］が、下記一般式［III］で表される、一分子中にＳｉＨ基を３個有するＳｉＨ基含有化合物（２）を含むことも好ましい。
(In the formula [II], R 3 is a monovalent group having 1 to 10 carbon atoms, an unsubstituted or substituted saturated hydrocarbon group or an aromatic hydrocarbon group, and may be the same or different in one molecule, a is an integer of 0 to 20, b is an integer of 0 to 20, and R 4 is a divalent organic group having 1 to 30 carbon atoms or an oxygen atom.)
When the rubber composition of the present invention contains a crosslinking agent [D], the crosslinking agent [D] is represented by the following general formula [III] and contains a SiH group-containing compound having three SiH groups in one molecule ( 2) is also preferably included.
本発明のハードディスクドライブは、前記本発明のゴム組成物からなるハードディスクドライブトップカバーガスケットを有する。
本発明の電線コネクター用シール材は、前記本発明のゴム組成物からなる。
The hard disk drive of the present invention has a hard disk drive top cover gasket made of the rubber composition of the present invention.
Electric wire connector sealing member of the present invention, the rubber composition of the present invention.
本発明の電線コネクターは、前記本発明のゴム組成物からなる電線コネクター用シール材を有する。前記本発明の電線コネクターは、自動車用電線コネクターであることが好ましい。 The electric wire connector of this invention has the sealing material for electric wire connectors which consists of a rubber composition of the said this invention. The electric wire connector of the present invention is preferably an automobile electric wire connector.
本発明のゴム組成物は、ＬＩＭ成形に好適であり、これを用いて成形された成形品は、シール性、耐熱性、耐酸性に優れ、低反力、低硬度であって、低温環境下でのシール性に寄与する低温回復性に優れるとともに、長期にわたって高温下での圧縮永久歪みが小さく、圧縮回復性に優れる。本発明のゴム組成物は、オイルブリードやブルームなどを生じず、機械的特性、耐アウトガス性に優れた成形品を製造することができ、電線コネクター用シールを成形した場合には電線のシール性と挿入性に優れたものとなり、燃料電池シール材、ＬＩＭ成形用ガスケット材、電線コネクター用シール材に好適である。本発明の燃料電池、ハードディスクドライブトップカバーガスケット、ハードディスクドライブ、電線コネクター等は、本発明のゴム組成物からなる成形体を具備しており、該成形体はシール性、耐熱性、耐酸性に優れ、低反力、低硬度であって、特に高温条件下での圧縮永久歪みが小さく、圧縮回復性に優れる。 The rubber composition of the present invention is suitable for LIM molding, and a molded product molded using the rubber composition is excellent in sealing property, heat resistance, acid resistance, low reaction force, low hardness and low temperature environment. In addition to being excellent in low-temperature recoverability that contributes to sealing performance at low temperature, compression set at high temperatures is small over a long period of time, and excellent in compression recovery. The rubber composition of the present invention does not produce oil bleed or bloom, and can produce a molded product having excellent mechanical properties and outgas resistance. When a wire connector seal is molded, the sealing property of the wire It has excellent insertability and is suitable for a fuel cell sealing material, a LIM molding gasket material, and a wire connector sealing material. The fuel cell, hard disk drive top cover gasket, hard disk drive, electric wire connector and the like of the present invention have a molded body made of the rubber composition of the present invention, and the molded body has excellent sealing properties, heat resistance and acid resistance. It has a low reaction force and a low hardness, has a small compression set particularly under high temperature conditions, and is excellent in compression recovery.
また、本発明で用いる表面改質シリカ［Ｃ］は、上記表面処理に加え、表面処理したことによるシリカ表面の立体障害を抑制するために、せん断破壊等の機械的処理を行ったものであってもよい。 In addition to the surface treatment, the surface-modified silica [C] used in the present invention has been subjected to mechanical treatment such as shear fracture in order to suppress steric hindrance on the silica surface due to the surface treatment. May be.
このようなシリカの表面改質処理度合は、Ｍ値で表され、本発明で用いる表面改質シリカ［Ｃ］はＭ値が５０以上であることが望ましい。なおＭ値は、シリカの表面改質処理度合を示す一般的な指標であって、測定対象となるシリカにメタノール水溶液のメタノール濃度を変えて添加した際、親和し始める（濡れ始める）時のメタノール水溶液濃度（メタノールのｖｏｌ％）で表される値である。 Such a surface modification treatment degree of silica is represented by an M value, and the surface-modified silica [C] used in the present invention desirably has an M value of 50 or more. The M value is a general index indicating the degree of surface modification treatment of silica. Methanol at the time of starting affinity (beginning to wet) when added to the silica to be measured while changing the methanol concentration of the methanol aqueous solution. It is a value represented by the aqueous solution concentration (vol% of methanol).
（式［II］中、Ｒ3は炭素数１〜１０の一価の基で、非置換あるいは置換の飽和炭化水素基または芳香族炭化水素基であり、１分子内で同種でも異種でもよく、ａは０〜２０の整数であり、ｂは０〜２０の整数であり、Ｒ4は炭素数１〜３０の二価の有機基または酸素原子である。） (In the formula [II], R 3 is a monovalent group having 1 to 10 carbon atoms, an unsubstituted or substituted saturated hydrocarbon group or an aromatic hydrocarbon group, and may be the same or different in one molecule, a is an integer of 0 to 20, b is an integer of 0 to 20, and R 4 is a divalent organic group having 1 to 30 carbon atoms or an oxygen atom.)
架橋剤［Ｄ］がＳｉＨ基含有化合物（２）を単独で含有すると、ゴム組成物は、三次元架橋し、機械強度などのゴム物性が向上する反面、回復性に劣るとともに、スコーチを起こしやすく成形時の取り扱い性が悪いなど、ゴム組成物を燃料電池シール材、ＬＩＭ成形用ガスケット材、電線コネクター用シール材などとして用いるには適当でない性状を示す場合がある点で改良の余地がある。 When the cross-linking agent [D] contains the SiH group-containing compound (2) alone, the rubber composition is three-dimensionally cross-linked to improve rubber physical properties such as mechanical strength, but is inferior in recoverability and easily causes scorch. such as poor handling property at the time of molding, the rubber composition of the fuel cell sealing member, LIM molding gasket material, for use as such electric wire connector sealing member there is room for improvement in that may exhibit properties not suitable.
架橋剤［Ｄ］がＳｉＨ基含有化合物（１）とＳｉＨ基含有化合物（２）とをともに含有すると、ゴム組成物は、成形性が良好で、耐熱性、バリア性、シール性に優れるとともに、高温時（１５０℃）における圧縮永久歪み率が低く、低温時（−３０℃）における弾性回復率（ＴＲ回復率）に優れ、燃料電池シール材、ＬＩＭ成形用ガスケット材、電線コネクター用シール材などの用途に好適に用いることができる。 When the crosslinking agent [D] contains both the SiH group-containing compound (1) and the SiH group-containing compound (2), the rubber composition has good moldability, excellent heat resistance, barrier properties, and sealing properties. at high temperatures (0.99 ° C.) compression set is low in excellent elastic recovery at low temperatures (-30 ° C.) (TR recovery ratio), the fuel cell sealing member, LIM molding gasket material, electric wire connector sealing member, etc. It can use suitably for the use of.
（ｉｉ）無機充填剤
無機充填剤の具体例としては、軽質炭酸カルシウム、重質炭酸カルシウム、タルク、クレー、ケイ藻土などが挙げられる。これらの無機充填剤は、単独であるいは２種以上組み合わせて用いることができる。これらの無機充填剤の種類および配合量は、その用途により適宜選択できるが、無機充填剤の配合量は通常、共重合体［Ａ］と必要に応じて添加されるその他の樹脂成分との合計１００重量部に対して、１〜最大３００重量部、好ましくは最大２００重量部である。
(Ii) Inorganic filler Specific examples of the inorganic filler include light calcium carbonate, heavy calcium carbonate, talc, clay, diatomaceous earth, and the like. These inorganic fillers can be used alone or in combination of two or more. The type and blending amount of these inorganic fillers can be appropriately selected depending on the use, but the blending amount of the inorganic filler is usually the sum of the copolymer [A] and other resin components added as necessary. The amount is 1 to 300 parts by weight, preferably 200 parts by weight, per 100 parts by weight.
本発明のハードディスクドライブトップカバーガスケットは、発泡などによる空隙を有さない、いわゆるボイドフリーであることが好ましい。
電線コネクター用シール材
本発明の電線コネクター用シール材は、上述の本発明のゴム組成物からなるものであって、例えば、固体高分子型（固体高分子電解質型）電線コネクター用シール材であることが好ましい。
The hard disk drive top cover gasket of the present invention is preferably so-called void-free, having no voids due to foaming or the like.
Electric wire connector sealing material for electric wire connector sealing member present invention, which consist of a rubber composition of the present invention described above, for example, a solid polymer electrolyte (solid polymer electrolyte) for electric wire connector sealing member It is preferable.
［実施例１］
エチレン・プロピレン・５−ビニル−２−ノルボルネンランダム共重合体（三井化学（株）製 ＰＸ−０６２、エチレン含量：５２．７重量％、ＶＮＢ含量：４．７重量％、２５℃における複素粘度（Anton Paar社（オーストラリア）製の粘弾性装置 ＭＣＲ３０１を用いて測定した複素粘度）：１１００Ｐａ・Ｓ、１３５℃のデカリン溶液中で測定した極限粘度［η］：０．２８ｄｌ／ｇ）１００重量部と、カーボンブラック（旭カーボン社製 旭＃５０ＨＧ、ヨウ素吸着量：１９ｍｇ／ｇ、平均粒子径８５ｎｍ、ＤＢＰ吸収量：１１０ｃｍ3／１００ｇ）１５重量部と、表面処理した沈殿法シリカ１（東ソー・シリカ社製Ｅ７５ＳＳ、ＢＥＴ表面積：５０ｍ2／ｇ、二次粒子径（コールターカウンター法により求めた平均粒子径）：２．４μｍ、Ｍ値：６５）３０重量部とを、容量２リットルのプラネタリーミキサー［（株）井上製作所製、商品名：ＰＬＭ−２型］で５０〜８０℃の範囲内で混練し、次いでこれに、老化防止剤として3-(3,5-ジ-t-ブチル-4-ヒドロキシ・フェニル)プロピオン酸ステアレート ０．４重量部（チバ・スペシャリティ・ケミカルズ製 Irganox １０７６）、触媒として白金−１，３，５，７−テトラビニルメチルシクロシロキサン錯体［白金濃度０．５重量％、末端ビニルシロキサンオイル溶液］０．４重量部、反応抑制剤として１−エチニル−１−シクロヘキサノール０．１重量部、下記式（１）で表される化合物（以下、架橋剤１という）を５重量部、および、下記式（２）で表される化合物（以下、架橋剤２という）を０．３重量部加えて、三本ロールミルにてゴム組成物を調製した。
[Example 1]
Ethylene / propylene / 5-vinyl-2-norbornene random copolymer (PX-062 manufactured by Mitsui Chemicals, Inc., ethylene content: 52.7% by weight, VNB content: 4.7% by weight, complex viscosity at 25 ° C. ( Viscoelasticity device manufactured by Anton Paar (Australia) (complex viscosity measured using MCR301): 1100 Pa · S, intrinsic viscosity [η] measured in decalin solution at 135 ° C .: 0.28 dl / g) 100 parts by weight , carbon black (Asahi carbon Co., Ltd. Asahi # 50HG, iodine adsorption: 19 mg / g, average particle size 85 n m, DBP absorption amount: 110cm 3 / 100g) and 15 parts by weight, precipitated silica and surface treated 1 (Tosoh E75SS manufactured by Silica, BET surface area: 50 m 2 / g, secondary particle diameter (average particle diameter determined by Coulter counter method): 2.4 μm, M value: 65) 30 parts by weight with a 2 liter planetary mixer [manufactured by Inoue Seisakusho Co., Ltd., trade name: PLM-2 type] in a range of 50 to 80 ° C. 0.4 part by weight of 3- (3,5-di-t-butyl-4-hydroxyphenyl) propionic acid stearate as an anti-aging agent (Irganox 1076 manufactured by Ciba Specialty Chemicals), and platinum-1,3 as a catalyst , 5,7-tetravinylmethylcyclosiloxane complex [platinum concentration 0.5% by weight, terminal vinylsiloxane oil solution] 0.4 part by weight, 1-ethynyl-1-cyclohexanol 0.1 part by weight as a reaction inhibitor, 5 parts by weight of a compound represented by the following formula (1) (hereinafter referred to as crosslinking agent 1) and 0.3 part by weight of a compound represented by the following formula (2) (hereinafter referred to as crosslinking agent 2) were added. To a three-roll mill The rubber composition was prepared.
なお、家庭向けの定置用燃料電池シール材としては９０℃４０，０００時間の性能が求められているが、研究の結果、１５０℃５００時間の評価で加速的に充分な評価ができることがわかった。すなわち、１５０℃５００時間で８０％未満であれば９０℃４０，０００時間の性能を満足できる。
（５）ＴＲ回復率
ＪＩＳ Ｋ６２６１に準拠して、−３０℃での低温弾性回復試験（ＴＲ試験）を行い、ＴＲ回復率を求めた。なお、回復率５５％以下では、低温性を満足できない。
（６）熱間特性（９０℃）
ＪＩＳ Ｋ６２５１に準拠して、測定温度９０℃、引張速度５００ｍｍ／分の条件で引張試験を行い、架橋シートの破断時の引張強度と伸びを測定した。なお、９０℃における破断伸びが２００％未満では、性能を満足させることはできない。
Although as a stationary fuel cell sealing member for the home has been required performance of 90 ° C. 40,000 hours, results of the study, found that it is accelerated to sufficient evaluation in the evaluation of 1 50 ° C. 500 hours It was. That is, if it is less than 80% at 150 ° C. for 500 hours, the performance at 90 ° C. for 40,000 hours can be satisfied.
(5) TR recovery rate In accordance with JIS K6261, a low temperature elastic recovery test (TR test) at -30 ° C was performed to obtain a TR recovery rate. If the recovery rate is 55% or less, the low temperature property cannot be satisfied.
(6) Hot characteristics (90 ° C)
In accordance with JIS K6251, a tensile test was performed under the conditions of a measurement temperature of 90 ° C. and a tensile speed of 500 mm / min, and the tensile strength and elongation at break of the crosslinked sheet were measured. In addition, if the elongation at break at 90 ° C. is less than 200%, the performance cannot be satisfied.
Claims (18)
（ａ）エチレンと、α−オレフィンと、非共役ポリエンとの共重合体であり、
（ｂ）α−オレフィンの炭素数が３〜２０であり、
（ｃ）エチレン単位／α−オレフィン単位の重量比が３５／６５〜９５／５であり、
（ｄ）よう素価が０．５〜５０の範囲であり、
（ｅ）１３５℃のデカリン溶液中で測定した極限粘度［η］が０．０１〜５．０ｄｌ／ｇである；
よう素吸着量が８０ｍｇ／ｇ以下であり、平均粒子径が２５０ｎｍ以下であり、かつ、ＤＢＰ吸収量が１０〜３００ｃｍ3／１００ｇであるカーボンブラック［Ｂ］と、
沈殿法シリカを表面改質して得られる、ＢＥＴ比表面積が３０〜８０ｍ2／ｇであり、
コールターカウンター法による粒子径が１．０〜４．０μｍであり、かつ、Ｍ値が５０以上である表面改質シリカ［Ｃ］と
を含有してなることを特徴とするゴム組成物。 An ethylene / α-olefin / non-conjugated polyene copolymer [A] satisfying the following (a) to (e):
(A) a copolymer of ethylene, α-olefin, and non-conjugated polyene;
(B) the α-olefin has 3 to 20 carbon atoms,
(C) The weight ratio of ethylene unit / α-olefin unit is 35/65 to 95/5,
(D) the iodine value is in the range of 0.5-50,
(E) the intrinsic viscosity [η] measured in a decalin solution at 135 ° C. is 0.01 to 5.0 dl / g;
Iodine adsorption of not more than 80 mg / g, an average particle diameter of at 250nm or less, and the carbon black [B] DBP absorption is 10~300cm 3 / 100g,
BET specific surface area obtained by surface modification of precipitation method silica is 30 to 80 m 2 / g,
A rubber composition comprising a surface-modified silica [C] having a particle size of 1.0 to 4.0 μm by a Coulter counter method and an M value of 50 or more.
（ｆ）非共役ポリエンが、下記の一般式［Ｉ］で表わされる少なくとも一種のノルボルネン化合物である。
０のアルキル基であり、Ｒ2は水素原子または炭素原子数１〜５のアルキル基である。） The rubber composition according to claim 1, wherein the ethylene / α-olefin / non-conjugated polyene copolymer [A] further satisfies the following (f):
(F) The non-conjugated polyene is at least one norbornene compound represented by the following general formula [I].
0 is an alkyl group, and R 2 is a hydrogen atom or an alkyl group having 1 to 5 carbon atoms. )
求項１〜４のいずれかに記載のゴム組成物。 Carbon black [B] is iodine adsorption amount 15~40mg / g, both the average particle diameter is 40 to 100 nm, of claims 1 to 4, DBP absorption and satisfies the 40~150cm 3 / 100g A rubber composition according to any one of the above.
基または芳香族炭化水素基であり、１分子内で同種でも異種でもよく、ａは０〜２０の整数であり、ｂは０〜２０の整数であり、Ｒ4は炭素数１〜３０の二価の有機基または酸素
原子である。）。 The rubber composition according to claim 6, wherein the crosslinking agent [D] contains a SiH group-containing compound (1) represented by the following general formula [II] and having two SiH groups in one molecule. object;
ｉＨ基含有化合物（２）を含むことを特徴とする請求項６または７に記載のゴム組成物；
The rubber composition according to claim 6 or 7, comprising an iH group-containing compound (2);
Priority Applications (7)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2007324439A JP5334409B2 (en) | 2006-12-26 | 2007-12-17 | Rubber composition and use thereof |
| CA2709416A CA2709416C (en) | 2007-12-17 | 2008-03-31 | Rubber composition and use thereof |
| KR1020107015736A KR101121263B1 (en) | 2007-12-17 | 2008-03-31 | Rubber composition and use thereof |
| US12/735,106 US8232341B2 (en) | 2007-12-17 | 2008-03-31 | Rubber composition and use thereof |
| EP08739428A EP2233528B1 (en) | 2007-12-17 | 2008-03-31 | Rubber composition and use thereof |
| PCT/JP2008/056314 WO2009078185A1 (en) | 2007-12-17 | 2008-03-31 | Rubber composition and use thereof |
| CN2008801205957A CN101896547B (en) | 2007-12-17 | 2008-03-31 | Rubber composition and use thereof |
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| JP2007324439A JP5334409B2 (en) | 2006-12-26 | 2007-12-17 | Rubber composition and use thereof |
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| JP2008179783A5 true JP2008179783A5 (en) | 2010-08-12 |
| JP5334409B2 JP5334409B2 (en) | 2013-11-06 |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010126668A (en) * | 2008-11-28 | 2010-06-10 | Nok Corp | Method for producing uncrosslinked rubber composition, and crosslinked rubber molded product |
| JPWO2011129168A1 (en) * | 2010-04-12 | 2013-07-11 | Nok株式会社 | Rubber composition and use thereof |
| JP5396337B2 (en) * | 2010-05-31 | 2014-01-22 | 東海ゴム工業株式会社 | Adhesive seal member for fuel cell |
| JP5729131B2 (en) * | 2010-06-02 | 2015-06-03 | 三井化学株式会社 | Crosslinkable rubber composition |
| JP6014971B2 (en) * | 2010-06-18 | 2016-10-26 | 東ソー株式会社 | Typical metal-containing polysiloxane composition, method for producing the same, and use thereof |
| JP5826111B2 (en) * | 2012-05-18 | 2015-12-02 | 三井化学株式会社 | Copolymer composition for screen printing |
| DE102013206266A1 (en) * | 2013-04-10 | 2014-10-16 | Wacker Chemie Ag | Crosslinkable compositions based on organosilicon compounds |
| JP6681247B2 (en) * | 2016-03-31 | 2020-04-15 | 住友理工株式会社 | Fuel cell seal member |
| JP7031620B2 (en) * | 2018-03-28 | 2022-03-08 | 豊田合成株式会社 | Manufacturing method of seal member for fuel cell and rubber composition for molding |
| US11084911B2 (en) | 2018-03-28 | 2021-08-10 | Toyoda Gosei Co., Ltd. | Method of producing sealing member for fuel cell and rubber composition for molding |
| JP7255476B2 (en) * | 2019-12-26 | 2023-04-11 | 豊田合成株式会社 | Brake hose and crosslinked rubber composition |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2762482B2 (en) * | 1988-10-07 | 1998-06-04 | 三井化学株式会社 | Method for producing higher α-olefin copolymer |
| JP3803173B2 (en) * | 1997-07-25 | 2006-08-02 | 三井化学株式会社 | Rubber composition for seal packing, seal packing and capacitor sealing seal comprising the composition |
| JP2000309709A (en) * | 1999-04-27 | 2000-11-07 | Kanegafuchi Chem Ind Co Ltd | Curable conductive composition and conductive rubber roller made by using it |
| JP4241383B2 (en) * | 2001-12-28 | 2009-03-18 | 三井化学株式会社 | Rubber composition for fuel cell seal parts, hard disk drive top cover gasket parts or seal parts for electric wire connectors and uses thereof |
| JP2005050666A (en) * | 2003-07-28 | 2005-02-24 | Tokai Rubber Ind Ltd | Hose material for fuel cell and hose for fuel cell using the same |
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2007
- 2007-12-17 JP JP2007324439A patent/JP5334409B2/en not_active Expired - Fee Related
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