JP2646926B2 - シリコーングリース - Google Patents

シリコーングリース

Info

Publication number
JP2646926B2
JP2646926B2 JP4030106A JP3010692A JP2646926B2 JP 2646926 B2 JP2646926 B2 JP 2646926B2 JP 4030106 A JP4030106 A JP 4030106A JP 3010692 A JP3010692 A JP 3010692A JP 2646926 B2 JP2646926 B2 JP 2646926B2
Authority
JP
Japan
Prior art keywords
group
silicone grease
silicone
mol
grease
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.)
Expired - Fee Related
Application number
JP4030106A
Other languages
English (en)
Other versions
JPH05194969A (ja
Inventor
孝行 高橋
元彦 平井
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shin Etsu Chemical Co Ltd
Original Assignee
Shin Etsu Chemical Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shin Etsu Chemical Co Ltd filed Critical Shin Etsu Chemical Co Ltd
Priority to JP4030106A priority Critical patent/JP2646926B2/ja
Priority to US08/006,286 priority patent/US5356549A/en
Publication of JPH05194969A publication Critical patent/JPH05194969A/ja
Application granted granted Critical
Publication of JP2646926B2 publication Critical patent/JP2646926B2/ja
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
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    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/50—Lubricating compositions characterised by the base-material being a macromolecular compound containing silicon
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    • C10M113/02—Carbon; Graphite
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    • C10M113/12—Silica
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    • C10M133/04—Amines, e.g. polyalkylene polyamines; Quaternary amines
    • C10M133/12—Amines, e.g. polyalkylene polyamines; Quaternary amines having amino groups bound to a carbon atom of a six-membered aromatic ring
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Description

【発明の詳細な説明】
【０００１】
【産業上の利用分野】本発明は、耐熱性及び耐寒性に優
れたシリコーングリースに関する。
【０００２】
【従来の技術及び発明が解決しようとする課題】シリコ
ーングリースはシリコーンオイルをベースオイルとし、
各種の増稠剤により増粘化し、必要に応じて添加剤を加
えてペースト状にしたものであり、ベースオイルとして
ジメチルシリコーンオイルを用いたシリコーングリース
が広く使用されている。
【０００３】しかし、ジメチルシリコーンオイルをベー
スオイルとするシリコーングリースは、−５０〜１７０
℃の温度範囲で使用可能で、耐寒性は良好であるものの
耐熱性は十分ではない。
【０００４】一方、耐熱性に優れるシリコーングリース
として、メチルフェニルシリコーンオイルやフロロシリ
コーンオイルをベースオイルとして用いたシリコーング
リースが知られており、これらの耐熱性は２００〜２５
０℃と優れるものの、耐寒性はせいぜい−３０℃止まり
である。
【０００５】このため耐熱性及び耐寒性の両特性を有す
るシリコーンオイルの開発が望まれている。
【０００６】本発明は上記事情に鑑みなされたもので、
耐熱性及び耐寒性に優れたシリコーングリースを提供す
ることを目的とする。
【０００７】
【課題を解決するための手段及び作用】本発明者は上記
目的を達成するため鋭意検討を行った結果、下記一般式
（１）で示され、アミン当量３７０００ｇ／モルを超え
２０万ｇ／モル以下、２５℃における粘度が１０〜１０
万センチストークス（ｃｓ）であるアミノ変性シリコー
ンオイルをベースオイルとして用いたシリコーングリー
スが−５０〜２００℃の範囲で使用可能であり、ジメチ
ルシリコーンオイルベースオイルとして用いた従来のシ
リコーングリースと同等の耐寒性を維持しつつ、耐熱性
を大幅に向上するものであることを知見し、本発明をな
すに至った。
【０００８】
【化２】 ［式中、Ｒ1は−Ｒ3−ＮＨ2又は−Ｒ3−ＮＨＲ4−ＮＨ2
で表される基（但し、Ｒ3，Ｒ4は同一又は異種の炭素数
１〜８のアルキレン基）、Ｒ2は炭素数１〜６の非置換
又は置換一価炭化水素基、ａ，ｂは０．０００１≦ａ≦
０．０１，１．９５≦ａ＋ｂ≦２．２０を満たす数であ
る。］
【０００９】以下、本発明を更に詳しく説明すると、本
発明のシリコーングリースは、（Ａ）上記一般式（１）
で示され、アミン等量３７０００ｇ／モルを超え２０万
ｇ／モル以下、２５℃における粘度が１０〜１０万ｃｓ
であるアミノ変性シリコーンオイルと（Ｂ）増稠剤とを
配合したものである。
【００１０】ここで、Ｒ1は−Ｒ3−ＮＨ2又は−Ｒ3−Ｎ
ＨＲ4−ＮＨ2で表される基であり、Ｒ3，Ｒ4は炭素数１
〜８、好ましくは炭素数２又は３のアルキレン基であ
り、Ｒ3とＲ4は同一でも異なっていてもよい。
【００１１】また、Ｒ2は炭素数１〜６の非置換又は置
換一価炭化水素基であり、ケイ素子に結合した形で分子
中に含まれる。このような一価炭化水素基として具体的
にはメチル基，エチル基，プロピル基，ブチル基，ヘキ
シル基等のアルキル基、シクロペンチル基，シクロヘキ
シル基等のシクロアルキル基、フェニル基，トリフロロ
プロピル基，ノナフロロヘキシル基等のハロゲン化アル
キル基などを挙げることができるが、特にメチル基が好
ましい。更にａ，ｂは０．０００１≦ａ≦０．０１、
１．９５≦ａ＋ｂ≦２．２０を満たす数である。ａが
０．０００１未満又は０．０１を超えた場合、得られる
シリコーングリースは耐熱性が劣るものとなってしま
う。
【００１２】また、上記式（１）で示されるアミノ変性
シリコーンオイルはアミノ基含有量がアミン当量で３７
０００ｇ／モルを超え２０万ｇ／モル以下の範囲である
が、好ましくは３７０００ｇ／モルを超え１５万ｇ／モ
ル以下の範囲である。アミン当量がこの範囲外の場合、
シリコーングリースは耐熱性が乏しいものとなってしま
う。
【００１３】上記アミノ変性シリコーンオイルの２５℃
での粘度は１０〜１０万であるが、より好ましくは２０
〜２万ｃｓの範囲である。粘度が１０ｃｓより低いとシ
リコーンオイルのグリース化に難点があり、また１０万
ｃｓを超えるとグリースの伸展性が乏しくなり、グリー
スとしての性能を発揮することができない場合がある。
【００１４】上記一般式（１）で示されるオルガノポリ
シロキサン（アミノ変性シリコーンオイル）は直鎖状、
分岐状及び環状のいずれであってもよいが、直鎖状のも
のが好適であり、特に好適なものとして下記平均組成式
（２）で示されるものが例示される。
【００１５】
【化３】 （式中、ｍは８〜１５００，ｎは０．００２〜３０の数
である。）
【００１６】上記式（２）で示されるシリコーンオイル
はそれ自体公知の方法で製造することができ、例えばト
リメチルシロキシ末端ポリジメチルシロキサン、オクタ
メチルシクロテトラシロキサン、メチルアミノプロピル
ポリシロキサンを原料とし、高温下で塩基性触媒を用い
て重合し、Ｎ2置換高温減圧ストリッピングで低分子シ
ロキサンを一定レベルまで除去することにより、容易に
製造することができる。
【００１７】（Ｂ）成分の増稠剤は本発明のシリコーン
グリースに所望の稠度を与えるもので、これには従来公
知の種々のものを使用することができる。具体的にはア
ルミニウム，鉛，亜鉛，マンガン，リチウム，ナトリウ
ム，カリウム，カルシウム，バリウム，ストロンチウ
ム，銅，水銀，ビスマス，クロム，鉄，ニッケル等の金
属を含有し、かつ炭素数が８個以上の脂肪酸の金属石ケ
ン、シリカ，アルミナ，酸化鉄，チタニア，酸化亜鉛，
ガラス繊維，粘土などの無機質微粒子活性酸化物、アリ
ール尿素、フタロシアニン、インダスレン、四弗化エチ
レン粉末、グラファイト、カーボンブラックなどが例示
される。このうちリチウムステアレート、リチウムヒド
ロキシステアレート、リチウムミリステート、リチウム
カプレートなどのリチウム石ケン類、四弗化エチレン粉
末、アリール尿素、シリカ、粘土などが特に好適に使用
される。
【００１８】（Ｂ）成分の配合量は（Ａ）成分１００部
（重量部、以下同じ）に対して２〜７０部、特に５〜６
５部とすることが好ましい。
【００１９】また、本発明のシリコーングリースには上
記（Ａ），（Ｂ）成分に加え必要に応じて各種成分を添
加することができる。このような成分として、シリコー
ングリースに酸化安定性を付与することを目的としたイ
ソプロポキシジフェニルアミン，４−メチレン−ビス−
２，６−ジターシャリーブチルフェノール等の酸化防止
剤、潤滑性向上を目的としたトリクレジルフォスフェー
ト等の極性添加剤、メチルリシノレート等の油性向上
剤、また、シリコーングリースの使用に際し、金属に与
える防錆を目的としたベンゾトリアゾール等の防錆剤な
どが挙げられる。
【００２０】本発明のシリコーングリースの製造方法
は、（Ａ）成分のオルガノポリシロキサンと（Ｂ）成分
の増稠剤を計量し、必要に応じて加熱し、プラネタリー
ミキサー等の混合機中で混合する。混合は窒素ガス等の
不活性ガス流通中で行うことが好ましい。
【００２１】混合後、均一仕上げのための混練り操作を
行う。混練り装置としては三本ロール、コロイドミル、
サンドグラインダー、ガウリンホモジナイザーなどが挙
げられるが、特に三本ロールを用いることが好ましい。
なお、上記各種成分を添加する場合、（Ａ）成分と
（Ｂ）成分との混合時に添加しても混合後の混練り時に
添加してもよい。
【００２２】
【実施例】以下、実施例と比較例を示し、本発明を具体
的に説明するが、本発明は下記の実施例に制限されるも
のではない。なお、各例中の粘度は２５℃における値を
示し、また、各例中の物性測定はＪＩＳ−Ｋ２２２０に
準じて行った。
【００２３】［実施例１、比較例１］
【００２４】
【化４】
【００２５】上記平均組成式（３）で表され、γ−アミ
ノプロピル基をアミン当量で９７０００ｇ／モル含有
し、粘度が３１１ｃｓのアミノ変性シリコーンオイル７
７０部、リチウムステアレート２３０部をプラネタリー
ミキサーを用い、１９５±５℃で１時間、窒素ガス流通
中で加熱混合した。冷却後、この混合物にイソプロポキ
シジフェニルアミン１部、メチルリシノレート５部、ト
リクレジルフォスフェート５部を加え、三本ロールを用
いて十分に混練りし、稠度（混和）２５０のシリコーン
グリースを得た（実施例１）。
【００２６】ベースオイルとして粘度が３００ｃｓのジ
メチルシリコーンオイルを用いた以外は実施例１と同様
にして稠度（混和）２５２のシリコーングリースを得た
（比較例１）。
【００２７】［実施例２、比較例２］
【００２８】
【化５】
【００２９】上記平均組成式（４）で表され、Ｎ−β
（アミノエチル）γ−アミノプロピル基をアミン当量で
１０００００ｇ／モル含有し、粘度が１００００ｃｓで
あるアミノ変性シリコーンオイル６５０部、四弗化エチ
レン粉末３５０部をプラネタリーミキサー中で十分混合
した後、三本ロールを用いて混練りし、稠度（混和）２
８５のシリコーングリースを得た（実施例２）。
【００３０】ベースオイルをとして粘度が１００００ｃ
ｓのジメチルシリコーンオイルを用いた以外は実施例２
と同様にして稠度（混和）２９０のシリコーングリース
を得た（比較例２）。
【００３１】
【００３２】
【００３３】
【００３４】
【００３５】［実施例３、比較例３］
【００３６】
【化７】
【００３７】上記平均組成式（５）で表され、Ｎ−β
（アミノエチル）γ−アミノプロピル基をアミン当量で
１０００００ｇ／モル含有し、粘度が３１５ｃｓである
アミノ変性シリコーンオイル７９０部、リチウムヒドロ
キシステアレート２１０部をプラネタリーミキサーを用
い、１９５±５℃で２時間、窒素ガス流通中で加熱混合
した。冷却後、この混合物に４，４メチレンビス２，６
ジターシャリーブチルフェノール１部、メチルリシノレ
ート５部、トリクレジルフォスフェート５部を加えて混
合した後、三本ロールを用いて混練りし、稠度（混和）
２５０のシリコーングリースを得た（実施例３）。
【００３８】ベースオイルとして粘度３００ｃｓのジメ
チルシリコーンオイルを用いた以外は実施例３と同様に
して稠度（混和）２４５のシリコーングリースを得た
（比較例３）。
【００３９】
【００４０】
【００４１】
【００４２】
【００４３】次に、実施例１〜３、比較例１〜３で得ら
れたグリースについて表１に示す物性を測定し、耐熱性
試験を行った。物性の測定はＪＩＳ−Ｋ−２２２０に準
じた方法で行い、耐熱性試験は２００℃熱風循環式恒温
中にグリースを放置し、５日後及び１０日後に１／４ス
ケールの稠度計カップ（三田村理研工業（株）製）を用
いて稠度を測定することにより行い、経時による稠度変
化を比較した。また、水洗耐水度はＪＩＳ−Ｋ２２２０
に準じて８０℃／１Ｈｒの試験条件により調べた。結果
を表１に併記する。
【００４４】
【表１】
【００４５】表１の結果から、ベースオイルとしてアミ
ノ変性シリコーンオイルを用いた本発明のシリコーング
リースは、ジメチルシリコーンオイルをベースとした従
来のシリコーングリースよりも耐熱性に優れることが確
認された。また、低温特性はジメチルシリコーンオイル
をベースオイルとしたグリースと同等に優れたものであ
った。
【００４６】
【発明の効果】本発明によれば、耐熱性及び耐寒性に優
れたシリコーングリースを得ることができる。
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ１０Ｎ 60:00

Claims (1)

    (57)【特許請求の範囲】
  1. 【請求項１】 （Ａ）下記一般式（１）で示され、アミ
    ン当量が３７０００ｇ／モルを超え２０万ｇ／モル以
    下、２５℃における粘度が１０〜１０万センチストーク
    スであるアミノ変性シリコーンオイル、 【化１】 ［式中、Ｒ１は−Ｒ３−ＮＨ２又は−Ｒ３−ＮＨＲ４−
    ＮＨ２で表される基（但し、Ｒ３，Ｒ４は同一又は異種
    の炭素数１〜８のアルキレン基）、Ｒ２は炭素数１〜６
    の非置換又は置換一価炭化水素基、ａ，ｂは０．０００
    １≦ａ≦０．０１，１．９５≦ａ＋ｂ≦２．２０を満た
    す数である。］ （Ｂ）増稠剤を配合してなることを特徴とするシリコー
    ングリース。
JP4030106A 1992-01-21 1992-01-21 シリコーングリース Expired - Fee Related JP2646926B2 (ja)

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JP4030106A JP2646926B2 (ja) 1992-01-21 1992-01-21 シリコーングリース
US08/006,286 US5356549A (en) 1992-01-21 1993-01-19 Silicone grease

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JP4030106A JP2646926B2 (ja) 1992-01-21 1992-01-21 シリコーングリース

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* Cited by examiner, † Cited by third party
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US6730380B2 (en) 1996-02-20 2004-05-04 Safeskin Corp. Readily-donned elastomeric articles
US20040122382A1 (en) * 2002-12-23 2004-06-24 Kimberly-Clark Worldwide, Inc. Elastomeric articles with beneficial coating on a surface
US7462661B2 (en) 2005-07-19 2008-12-09 Xerox Corporation Release fluid additives
CN100543104C (zh) * 2005-12-16 2009-09-23 富准精密工业(深圳)有限公司 导热膏及使用该导热膏的电子装置
JP5517174B2 (ja) * 2009-07-27 2014-06-11 ヒュンダイ スチール カンパニー 連続鋳造スラブの中心偏析評価方法
US8652400B2 (en) 2011-06-01 2014-02-18 Ati Properties, Inc. Thermo-mechanical processing of nickel-base alloys
US20150261260A1 (en) * 2013-03-15 2015-09-17 Royce J. Nicholas Method of water-proofing electronic components
CN109652167A (zh) * 2018-12-20 2019-04-19 新协同（宁波）油脂有限公司 一种用于燃气旋塞阀的润滑脂及其制备方法

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JPS6291560A (ja) * 1985-10-18 1987-04-27 Asahi Glass Co Ltd 潤滑性樹脂組成物
JPS63275696A (ja) * 1987-05-07 1988-11-14 Shin Etsu Chem Co Ltd シリコ−ングリ−ス組成物
JP2793228B2 (ja) * 1989-02-27 1998-09-03 日本ケーブル・システム株式会社 コントロールケーブル用潤滑剤およびそれを用いてなるコントロールケーブル

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