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JP3670361B2 - Grease composition for constant velocity joints - Google Patents

Grease composition for constant velocity joints Download PDF

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Publication number
JP3670361B2
JP3670361B2 JP25898295A JP25898295A JP3670361B2 JP 3670361 B2 JP3670361 B2 JP 3670361B2 JP 25898295 A JP25898295 A JP 25898295A JP 25898295 A JP25898295 A JP 25898295A JP 3670361 B2 JP3670361 B2 JP 3670361B2
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JP
Japan
Prior art keywords
group
mass
extreme pressure
sulfur
pressure agent
Prior art date
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Expired - Lifetime
Application number
JP25898295A
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Japanese (ja)
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JPH09100488A (en
Inventor
広嗣 木下
宗市 野村
優 三嶋
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.)
Eneos Corp
Original Assignee
Nippon Oil Corp
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Priority to JP25898295A priority Critical patent/JP3670361B2/en
Priority to EP96115965A priority patent/EP0767237A1/en
Publication of JPH09100488A publication Critical patent/JPH09100488A/en
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Publication of JP3670361B2 publication Critical patent/JP3670361B2/en
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  • Chemical Kinetics & Catalysis (AREA)
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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Lubricants (AREA)

Description

【0001】
【発明の属する技術分野】
本発明は固定型ジョイント及びスライド型ジョイントである等速ジョイント用グリース組成物に関する。
【0002】
【従来の技術】
一般に、FF車において、等速ジョイントを適用する場合には、(固定型ジョイント)+(シャフト)+(スラスト型ジョイント)の組み合わせで使用されている。
【0003】
固定型ジョイントには、バーフィールドジョイント、ゼッパジョイント、アンダーカットフリージョイント及びトリポードジョイント等があり、スライド型ジョイントにはダブルオフセットジョイント、トリポードジョイント及びクロスグルーブジョイント等がある。
【0004】
これらの等速ジョイントに封入使用される潤滑剤としては、従来から精製鉱油とリチウム石けんやウレア系増ちょう剤とからなる基グリースに、二硫化モリブデン、鉛系化合物等を組み合わせた極圧グリースが主に使用されている。
【0005】
等速ジョイント用グリースには、(1)耐フレーキング性、(2)耐焼付き性、(3)耐摩耗性、(4)低摩擦性等の性能が要求される。しかし、最近の自動車の高性能化、高級化傾向に対して従来のグリースでは性能不足となってきており、特に等速ジョイントの寿命延長の面から、耐フレーキング性能の向上が切望されている。
【0006】
【発明が解決しようとする課題】
本発明の目的は、特に耐フレーキング性能に優れ、等速ジョイントの寿命を延命させることができる等速ジョイント用グリース組成物を提供することにある。
【0007】
【課題を解決するための手段】
本発明によれば、基油に、組成物全量を基準として、
(1)増ちょう剤2〜25質量%、
(2)窒化ホウ素粉体0.5〜20質量%、及び
(3)極圧剤として、硫黄−リン系極圧剤0.1〜10質量%
を含有し、前記硫黄−リン系極圧剤が
(3−1)硫黄系極圧剤及びリン系極圧剤の混合物であって、前記硫黄系極圧剤が硫化油脂、硫黄架橋された金属フェネート、ジヒドロカルビルポリサルファイド、ジチオカーバメート類、モノスルフィド、スルホキシド、スルフィネート及びこれらの混合物から選ばれる硫黄系極圧剤であり、前記リン系極圧剤がホスフェート、ホスファイト、ホスフィネート、ホスホネート、これらのアミン塩及びこれらの混合物の中から選ばれるリン系極圧剤である混合物であることを特徴とする等速ジョイント用グリース組成物が提供される。
【0008】
【発明の実施の形態】
本発明の等速ジョイント用グリース組成物の基油としては、鉱油及び/又は合成油を好ましく挙げることができる。前記鉱油としては、石油精製業の潤滑油製造プロセスで通常行われている方法により得られる、たとえば、原油を常圧蒸留及び減圧蒸留して得られた潤滑油留分を溶剤脱れき、溶剤抽出、水素化分解、溶剤脱ろう、接触脱ろう、水素化精製、硫酸洗浄、白土処理等の処理を1つ以上行って精製したものが挙げられる。
【0009】
また、前記合成油の具体例としては、ポリブテン、1−オクテンオリゴマー、1−デセンオリゴマー等のポリα−オレフィン又はこれらの水素化物;ジトリデシルグルタレート、ジ−2−エチルヘキシルアジペート、ジイソデシルアジペート、ジトリデシルアジペート、ジ−3−エチルヘキシルセバケート等のジエステル;トリメチロールプロパンカプリレート、トリメチロールプロパンペラルゴネート、ペンタエリスリトール−2−エチルヘキサノエート、ペンタエリスリトールペラルゴネート等のポリオールエステル;アルキルナフタレン;アルキルベンゼン;ポリオキシアルキレングリコール;ポリフェニルエーテル;ジアルキルジフェニルエーテル;シリコーン油;パーフルオロアルキルエーテル等を挙げることができ、使用に際しては単独若しくは混合物として用いることができる。
【0010】
これらの基油の粘度範囲は通常使用されている潤滑油の粘度範囲であるならばすべて使用可能であるが、100℃での動粘度として通常2〜40mm2/s、好ましくは3〜20mm2/sであることが望ましい。また基油の粘度指数は好ましくは90以上、さらに好ましくは100以上であることが望ましい。
【0011】
本発明の等速ジョイント用グリース組成物は、必須成分として増ちょう剤を含む。前記増ちょう剤としては金属石けん、複合金属石けん等の石けん系;ベントン、シリカゲル、ウレア化合物、ウレア・ウレタン化合物、ウレタン化合物等の非石けん系等、あらゆる増ちょう剤が使用可能であるが、耐熱性の点からウレア化合物、ウレア・ウレタン化合物、ウレタン化合物又はこれらの混合物等が好ましい。
【0012】
前記石けん系増ちょう剤としては、例えばナトリウム石けん、カルシウム石けん、アルミニウム石けん、リチウム石けん等が挙げられる。
【0013】
また前記ウレア化合物、ウレア・ウレタン化合物及びウレタン化合物としては、例えばジウレア化合物、トリウレア化合物、テトラウレア化合物、その他のポリウレア化合物、ウレア・ウレタン化合物、ジウレタン化合物又はこれらの混合物等が挙げられる。更に好ましくは、前記ジウレア化合物、ウレア・ウレタン化合物、ジウレタン化合物又はこれらの混合物を挙げることができ、更に具体的には、例えば下記一般式(1)で表される化合物単独若しくはこれらの混合物が好ましい。
【0014】
【化1】

Figure 0003670361
【0015】
前記一般式(1)中のR1は好ましくは炭素数6〜20、特に好ましくは炭素数6〜15の2価の炭化水素基である。前記2価の炭化水素基としては、直鎖又は分枝アルキレン基、直鎖又は分枝アルケニレン基、シクロアルキレン基、芳香族基等が挙げられる。R1の具体例としてはエチレン基、2,2−ジメチル−4−メチルへキシレン基、下記式(a)〜(j)で表される基を挙げることができる。
【0016】
【化2】
Figure 0003670361
【0017】
【化3】
Figure 0003670361
【0018】
これらの中でも、(d)及び(e)が特に好ましい。
【0019】
また前記一般式(1)中のR2、R3、R4及びR5としては、直鎖又は分枝アルキル基、直鎖又は分枝アルケニル基、シクロアルキル基、アルキルシクロアルキル基、アリール基、アルキルアリール基、アリールアルキル基等が挙げられる。具体的には例えば、ヘキシル基、ヘプチル基、オクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基、ノナデシル基、エイコシル基等の直鎖又は分枝アルキル基;ヘキセニル基、ヘプテニル基、オクテニル基、ノネニル基、デセニル基、ウンデセニル基、ドデセニル基、トリデセニル基、テトラデセニル基、ペンタデセニル基、ヘキサデセニル基、ヘプタデセニル基、オクタデセニル基、ノナデセニル基、エイコセニル基等の直鎖又は分枝アルケニル基;シクロヘキシル基;メチルシクロヘキシル基、ジメチルシクロヘキシル基、エチルシクロヘキシル基、ジエチルシクロヘキシル基、プロピルシクロヘキシル基、イソプロピルシクロヘキシル基、1−メチル−3−プロピルシクロヘキシル基、ブチルシクロヘキシル基、アミルシクロヘキシル基、アミルメチルシクロヘキシル基、ヘキシルシクロヘキシル基、ヘプチルシクロヘキシル基、オクチルシクロヘキシル基、ノニルシクロヘキシル基、デシルシクロヘキシル基、ウンデシルシクロヘキシル基、ドデシルシクロヘキシル基、トリデシルシクロヘキシル基、テトラデシルシクロヘキシル基等のアルキルシクロアルキル基;フェニル基、ナフチル基等のアリール基;トルイル基、エチルフェニル基、キシリル基、プロピルフェニル基、クメニル基、メチルナフチル基、エチルナフチル基、ジメチルナフチル基、プロピルナフチル基等のアルキルアリール基;ベンジル基、メチルベンジル基、エチルベンジル基等のアリールアルキル基等を挙げることができ、これらの中でもシクロヘキシル基、オクタデシル基及びトルイル基が特に好ましい。
【0020】
前記ジウレア化合物、ウレア・ウレタン化合物又はジウレタン化合物を製造するには、例えば、一般式OCN−R1−NCOで表されるジイソシアネートと、一般式R2NH2、R34NH又はR5OHで表される化合物若しくはこれらの混合物とを、基油中で10〜200℃で反応させることにより得られる。この際R1、R2、R3、R4及びR5は、前記一般式(1)のR1、R2、R3、R4及びR5と同一である。
【0021】
前記増ちょう剤の含有量は、グリース組成物全量を基準として、2〜25質量%、好ましくは3〜20質量%である。増ちょう剤の含有量が2質量%未満の場合は増ちょう剤としての効果が少ないため十分なグリース状とはならず、また25質量%を越えるとグリースとして硬くなりすぎて十分な潤滑性能を発揮することができない。
【0022】
本発明のグリース組成物は、必須成分として窒化ホウ素粉体を含む。前記窒化ホウ素粉体の粒径については特に限定はないが、平均粒径は通常0.05〜20μm、好ましくは0.4〜15μm、さらに好ましくは5〜10μmであることが望ましい。
【0023】
前記窒化ホウ素粉体の含有量は、グリース組成物全量を基準として、0.5〜20質量%、好ましくは1〜20質量%である。窒化ホウ素粉体の含有量が0.5質量%未満の場合は耐フレーキング性能に支障が生じ、また等速ジョイントの焼付き寿命が不十分となる。また窒化ホウ素粉体の含有量が20質量%を越えるとざらつき摩耗(粒子の研削作用による摩耗)が促進してしまい、また等速ジョイントの寿命が不十分となる。
【0024】
本発明のグリース組成物は、必須成分として硫黄−リン系極圧剤を含む。
【0025】
前記硫黄−リン系極圧剤とは、硫黄のみを含有する硫黄系極圧剤、及びリンのみを含有するリン系極圧剤の混合物である。
【0026】
前記硫黄−リン系極圧剤中の硫黄原子とリン原子の比率は100:25〜100:1の範囲であることが好ましい。
【0027】
前記硫黄系極圧剤とは、硫化油脂、硫黄架橋された金属フェネート、ジヒドロカルビルポリサルファイド、ジチオカーバメート類、モノスルフィド、スルホキシド、スルフィネート及びこれらの混合物の中から選ばれる硫黄系極圧剤である。これらの中でも硫化油脂、ジヒドロカルビルポリサルファイド、又はこれらの混合物が好ましい。
【0028】
前記硫化油脂とは、オリーブ油、ヒマシ油、茶実油、ヌカ油、綿実油、ナタネ油、トウモロコシ油、牛脂、牛脚油、マッコウ鯨油、鯨ロウ等、不飽和結合を有する動植物油脂に硫黄を加え、加熱することにより得られる化合物をいう。前記硫化油脂の硫黄含有量は通常5〜15質量%、好ましくは8〜12質量%であることが望ましい。
【0029】
また前記硫黄架橋された金属フェネートとしては炭素数8〜30、好ましくは9〜20のアルキル基が付加されたアルキルフェノールの硫化物のアルカリ土類金属塩等が挙げられる。前記アルキル基の具体例としてはオクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基、ノナデシル基、イコシル基、ヘンイコシル基、ドコシル基、トリコシル基、テトラコシル基、ペンタコシル基、ヘキサコシル基、ヘプタコシル基、オクタコシル基、ノナコシル基、トリアコンチル基等が挙げられ、これらは直鎖状でも分枝状でもよい。前記アルキル基としてはノネン、炭素数5〜8のオレフィン又はアルコールから誘導されるものが好ましい。またアルカリ土類金属としてはマグネシウム、カルシウム又はバリウムが好ましい。
【0030】
また前記ジヒドロカルビルポリサルファイドとは下記一般式(2)で表される化合物を意味する。
【0031】
【化4】
Figure 0003670361
【0032】
式中、R6及びR7は同一又は異なる基であって、プロピレン又はイソブテンから誘導された炭素数3〜18、好ましくは6〜15のアルキル基、あるいは炭素数6〜8のアリール基、アルキルアリール基又はアリールアルキル基であることが好ましく、これらの基としては例えば、イソプロピル基、プロピレン2量体から誘導される分枝ヘキシル基、プロピレン3量体から誘導される分枝ノニル基、プロピレン4量体から誘導される分枝ドデシル基、プロピレン5量体から誘導される分枝ペンタデシル基、プロピレン6量体から誘導される分枝オクタデシル基、tert−ブチル基、イソブテン2量体から誘導される分枝オクチル基、イソブテン3量体から誘導される分枝ドデシル基、イソブテン4量体から誘導される分枝ヘキサデシル基等のアルキル基(これらのアルキル基は全ての分枝異性体を含む。);フェニル基、トリル基、エチルフェニル基、キシリル基等のアルキルアリール基(これらアルキルアリール基のアルキル部分は直鎖でも分枝でもよく、アルキル部分のアリール基上の置換位置は任意である。);又はベンジル基、フェニルエチル基(フェニル基の置換位置は任意である。)等のアリールアルキル基等が挙げられる。
【0033】
一般式(2)中のzは1〜5、好ましくは2〜4の数を示す。また、zが3以上の場合は、
【0034】
【化5】
Figure 0003670361
【0035】
のように環を形成していてもよい。
【0036】
前記ジヒドロカルビルポリサルファイドの具体例としては、ジブチルポリサルファイド、ジヘキシルポリサルファイド、ジオクチルポリサルファイド、ジノニルポリサルファイド、ジデシルポリサルファイド、ジドデシルポリサルファイド、ジテトラデシルポリサルファイド、ジヘキサデシルポリサルファイド、ジオクタデシルポリサルファイド、ジエイコシルポリサルファイド、ジフェニルポリサルファイド、ジベンジルポリサルファイド、ジフェネチルポリサルファイド、ポリプロペニルポリサルファイド、ポリブテニルポリサルファイド又はこれらの混合物等が挙げられるが、特にポリプロペニルポリサルファイド、ポリブテニルポリサルファイド又はこれらの混合物が好ましい。
【0037】
前記ポリプロペニルポリサルファイド、ポリブテニルポリサルファイド又はこれらの混合物は、プロピレン、イソブテン、これら単量体の2〜4量体、あるいはこれら単量体又は重合体の混合物等のオレフィン性炭化水素を元素硫黄、ハロゲン化硫黄(例えば、1塩化硫黄又は2塩化硫黄)、硫化水素又はこれらの混合物等により硫化することによって得ることができる。
【0038】
前記ジヒドロカルビルポリサルファイドの硫黄含有量は通常30〜50質量%、好ましくは40〜45質量%であることが望ましい。
【0039】
また前記ジチオカーバメート類としては、次の一般式(3)で表されるアルキルチオカルバミル化合物が挙げられる。
【0040】
【化6】
Figure 0003670361
【0041】
式中R8、R9、R10及びR11は同一又は異なる基であって、それぞれ炭素数1〜18、好ましくは1〜10の直鎖又は分枝アルキル基を表し、具体的には、メチル基、エチル基、プロピル基、n−ブチル基、イソブチル基、ペンチル基、イソペンチル基、ヘキシル基、ヘプチル基、オクチル基、2−エチルヘキシル基、ノニル基、デシル基、トリデシル基又はオクタデシル基等のアルキル基を挙げることができる。
【0042】
また式中(Y)はS、S−S、S−CH2−S、S−(CH22−S、S−(CH23−S、あるいはS−Zn−Sを表す。
【0043】
前記アルキルジチオカルバミル化合物の具体的な例としては、メチレンビス(ジブチルジチオカーバメート)、ビス(ジメチルチオカルバミル)モノスルフィド、ビス(ジメチルチオカルバミル)ジスルフィド、ビス(ジブチルチオカルバミル)ジスルフィド、ビス(ジペンチルチオカルバミル)ジスルフィド、ビス(ジオクチルチオカルバミル)ジスルフィド、亜鉛ジペンチルジチオカーバメート等を挙げることができる。
【0044】
前記リン系極圧剤とは、ホスフェート、ホスファイト、ホスフィネート、ホスホネート、これらのアミン塩及びこれらの混合物から選ばれるリン系極圧剤である。これらの中でも、ホスフェート、ホスファイト又はこれらの混合物が好ましい。
【0045】
ここでいうホスフェートとは下記一般式(4)で表される化合物を、ホスファイトとは下記一般式(5)で表される化合物をそれぞれ示す。
【0046】
【化7】
Figure 0003670361
【0047】
【化8】
Figure 0003670361
【0048】
式中、R12は炭素数1〜24のアルキル基、シクロアルキル基、アルキルシクロアルキル基、アルケニル基、アリール基、アルキルアリール基又はアリールアルキル基等を、R13及びR14は水素原子、炭素数1〜24のアルキル基、シクロアルキル基、アルキルシクロアルキル基、アルケニル基、アリール基、アルキルアリール基又はアリールアルキル基等をそれぞれ示す。
【0049】
12、R13及びR14の水素原子以外の具体例としてはメチル基、エチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、ノニル基、デシル基、ドデシル基、テトラデシル基、ヘキサデシル基、オクタデシル基、エイコシル基、ドコシル基、テトラコシル基、シクロペンチル基、シクロヘキシル基、メチルシクロヘキシル基、エチルシクロヘキシル基、ジメチルシクロヘキシル基、シクロヘプチル基、フェニル基、トリル基、キシリル基、エチルフェニル基、プロピルフェニル基、ブチルフェニル基、ペンチルフェニル基、ヘキシルフェニル基、ノニルフェニル基、デシルフェニル基、ドデシルフェニル基、テトラデシルフェニル基、ヘキサデシルフェニル基、オクタデシルフェニル基、ベンジル基又はフェネチル基等を挙げることができる。
【0050】
前記リン系極圧剤の具体例としてはトリブチルホスフェート、ベンジルジフェニルホスフェート、エチルジフェニルホスフェート、オクチルジフェニルホスフェート、トリフェニルホスフェート、トリクレジルホスフェート、トリトリルホスフェート、2−エチルヘキシルジフェニルホスフェート、トリブチルホスファイト、ジラウリルホスファイト等が挙げられる。
【0051】
前記硫黄系極圧剤及び前記リン系極圧剤の併用は、前記ジヒドロカルビルポリサルファイドと前記ホスフェートとの併用、又は前記硫化油脂と前記ホスフェートとの併用が特に好ましい。
【0053】
本発明のグリース組成物における硫黄−リン系極圧剤の含有量は、グリース組成物全量基準で、0.1〜10質量%、好ましくは1〜5質量%である。硫黄−リン系極圧剤の含有量が0.1質量%未満の場合は等速ジョイントの焼付き寿命が不十分となる。また硫黄−リン系極圧剤の含有量が10質量%を越えると添加量に見合った性能が得られず不経済である。
【0054】
本発明の等速ジョイント用グリース組成物は、極圧剤として、前記硫黄−リン系極圧剤に加え、さらにモリブデンジチオカーバメートを含有することができる。
【0055】
前記モリブデンジチオカーバメートとしては下記一般式(6)で表されるものが挙げられる。
【0056】
【化9】
Figure 0003670361
【0057】
式中、R15、R16、R17及びR18はそれぞれ同一又は異なる基であって、アルキル基、アルケニル基、アリール基、アルキルアリール基、アリールアルキル基等の炭化水素基を示し、特にアルキル基が好ましい。
【0058】
15、R16、R17及びR18の具体例としてはエチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基等の炭素数2〜18、好ましくは8〜13の直鎖又は分枝アルキル基;ブチルフェニル基、ノニルフェニル基等のアルキルアリール基等が挙げられる。またX1、X2、X3及びX4はそれぞれ硫黄原子又は酸素原子を示す。
【0059】
前記モリブデンジチオカーバメートの具体例としては硫化モリブデンジエチルジチオカーバメート、硫化モリブデンジプロピルジチオカーバメート、硫化モリブデンジブチルジチオカーバメート、硫化モリブデンジペンチルジチオカーバメート、硫化モリブデンジヘキシルジチオカーバメート、硫化モリブデンジオクチルジチオカーバメート、硫化モリブデンジデシルジチオカーバメート、硫化モリブデンジドデシルジチオカーバメート、硫化モリブデンジトリデシルジチオカーバメート、硫化モリブデンジ(ブチルフェニル)ジチオカーバメート、硫化モリブデンジ(ノニルフェニル)ジチオカーバメート、硫化オキシモリブデンジエチルジチオカーバメート、硫化オキシモリブデンジプロピルジチオカーバメート、硫化オキシモリブデンジブチルジチオカーバメート、硫化オキシモリブデンジペンチルジチオカーバメート、硫化オキシモリブデンジヘキシルジチオカーバメート、硫化オキシモリブデンジオクチルジチオカーバメート、硫化オキシモリブデンジデシルジチオカーバメート、硫化オキシモリブデンジドデシルジチオカーバメート、硫化オキシモリブデンジトリデシルジチオカーバメート、硫化オキシモリブデンジ(ブチルフェニル)ジチオカーバメート、硫化オキシモリブデンジ(ノニルフェニル)ジチオカーバメート等を挙げることができる。これらの各化合物は単独又は混合物として使用することができる。
【0060】
本発明のグリース組成物における前記モリブデンジチオカーバメートの含有量は、グリース組成物全量基準で、通常0.1〜10質量%、好ましくは1〜5質量%であることが望ましい。
【0061】
また前記モリブデンジチオカーバメートと前記硫黄−リン系極圧剤とを併用する場合の重量比率はモリブデンジチオカーバメート:硫黄−リン系極圧剤が通常1:5〜5:1、好ましくは1:3〜3:1であることが望ましい。
【0062】
また、本発明のグリース組成物にさらに有機亜鉛化合物を添加することにより、さらに耐フレーキング性能を向上させることができる。前記有機亜鉛化合物としては例えば、ジチオリン酸亜鉛、ジチオカルバミン酸亜鉛、脂肪酸亜鉛塩、ナフテン酸亜鉛塩等が使用できる。
【0063】
前記ジチオリン酸亜鉛としては下記一般式(7)で表される化合物が挙げられる。
【0064】
【化10】
Figure 0003670361
【0065】
式中、R19、R20、R21及びR22は同一又は異なる基であって、それぞれ炭素数2〜18の直鎖又は分枝の1級又は2級アルキル基、アリール基又はアリールアルキル基を示し、具体的にはエチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基等が挙げられる。
【0066】
また、前記ジチオカルバミン酸亜鉛としては下記一般式(8)で表される化合物が挙げられる。
【0067】
【化11】
Figure 0003670361
【0068】
式中、R23、R24、R25及びR26は同一又は異なる基であって、それぞれ炭素数2〜18のアルキル基、アルケニル基、アリール基、アルキルアリール基又はアリールアルキル基を示し、具体的にはエチル基、プロピル基、ブチル基、ペンチル基、ヘキシル基、ヘプチル基、オクチル基、ノニル基、デシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基等のアルキル基(これらアルキル基は直鎖でも分枝でもよく、また1級でも2級でもよい。);ブチルフェニル基、ノニルフェニル基等のアルキルアリール基(これらアルキルアリール基のアルキル部分は直鎖でも分枝でもよく、アルキル部分のアリール基上の置換位置は任意である。)等が挙げられる。
【0069】
前記脂肪酸亜鉛塩としては下記一般式(9)で表される化合物が挙げられる。
【0070】
【化12】
Figure 0003670361
【0071】
式中、R27は炭素数3〜22のアルキル基又はアルケニル基を表す。
【0072】
前記ナフテン酸亜鉛塩としては下記一般式(10)で表される化合物が挙げられる。
【0073】
【化13】
Figure 0003670361
【0074】
式中、R28はシクロペンチル基、シクロヘキシル基、アルキルシクロペンチル基、アルキルシクロヘキシル基等のシクロアルキル基を示し、mは整数を示す。
【0075】
本発明のグリース組成物に有機亜鉛化合物を含有させる場合の含有量は、グリース組成物全量基準で、通常0.1〜10質量%、好ましくは1〜5質量%であることが望ましい。
【0076】
なお、本発明の等速ジョイント用グリース組成物では、その性質を損ねることがない限り、さらに性能を向上させるために必要に応じて固体潤滑剤;硫黄−リン系やモリブデンジチオカーバメート以外の他の極圧剤;酸化防止剤;油性剤;さび止め剤;粘度指数向上剤等の他の添加物を含有させることができる。
【0077】
前記固体潤滑剤としては具体的には例えば、黒鉛、フッ化黒鉛、ポリテトラフロロエチレン、二硫化モリブデン、硫化アンチモン、アルカリ(土類)金属ホウ酸塩等が挙げられる。
【0078】
前記他の極圧剤としては具体的には、塩素化パラフィン、塩素化エステル等の塩素系化合物;モリブデンジチオホスフェート等のモリブデン化合物等が挙げられる。
【0079】
前記酸化防止剤としては具体的には、2,6−ジ−t−ブチルフェノール、2,6−ジ−t−ブチル−p−クレゾール等のフェノール系化合物、ジアルキルジフェニルアミン、フェニル−α−ナフチルアミン、p−アルキルフェニル−α−ナフチルアミン等のアミン系化合物、硫黄系化合物、フェノチアジン系化合物等が挙げられる。
【0080】
前記油性剤としては具体的には、ラウリルアミン、ミリスチルアミン、パルミチルアミン、ステアリルアミン、オレイルアミン等のアミン類;ラウリルアルコール、ミリスチルアルコール、パルミチルアルコール、ステアリルアルコール、オレイルアルコール等の高級アルコール;ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、オレイン酸等の高級脂肪酸;ラウリン酸メチル、ミリスチン酸メチル、パルミチン酸メチル、ステアリン酸メチル、オレイン酸メチル等の脂肪酸エステル;ラウリルアミド、ミリスチルアミド、パルミチルアミド、ステアリルアミド、オレイルアミド等のアミド類;油脂等が挙げられる。
【0081】
前記さび止め剤としては具体的には、金属石けん;石油スルホネート、アルキルベンゼンスルホネート、ジノニルナフタレンスルホネート等の合成スルホネート;ソルビタン脂肪酸エステル等の多価アルコール部分エステル;アミン;リン酸;リン酸塩等が挙げられる。
【0082】
前記粘度指数向上剤としては具体的には、ポリメタクリレート、ポリイソブチレン、ポリスチレン等が挙げられる。
【0083】
本発明の等速ジョイント用グリース組成物を調製するには、例えば前記基油に、前記増ちょう剤、前記窒化ホウ素粉体、前記硫黄−リン系極圧剤、また必要に応じて前記モリブデンジチオカーバメート、前記有機亜鉛化合物又は前記他の添加物を撹拌し、ロールミル等を通すことにより得ることができる。また前記基油に増ちょう剤の原料成分を予め添加、溶融し、撹拌混合させて、前記増ちょう剤を調製すると同時に、本発明のグリース組成物を製造することもできる。
【0084】
【発明の効果】
本発明の等速ジョイント用グリース組成物は、耐フレーキング性能に優れ、等速ジョイントの寿命を延命させることができる。
【0085】
【実施例】
以下本発明の内容を、実施例及び比較例によりさらに具体的に説明するが、本発明はこれらに限定されるものではない。
【0086】
【実施例1】
ジフェニルメタン−4,4’−ジイソシアネート88.0gを350gの鉱油に入れ、60℃に加熱し、均一に溶解させた。次いでドデシルアルコール26.2gを同鉱油200gに加熱溶解させた溶解物を添加し、激しく攪拌した後、さらにシクロヘキシルアミン55.8gを同鉱油205gに溶解させた溶解物を加え、再度激しく攪拌したところ、ゲル状物質が生じた。攪拌を続けながら100℃にて30分間保持した後、増ちょう剤、窒化ホウ素粉体及び極圧剤を含む添加剤を添加して撹拌し、3本ロールミルを通して目的のグリース組成物を調製した。得られたグリース組成物につき、以下の方法で評価試験を行った。その結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0087】
組成
増ちょう剤 17.0質量%
鉱油(126mm2/s@40℃) 77.5質量%
窒化ホウ素粉体(平均粒径:0.7μm) 1.5質量%
硫化油脂(硫黄含有量9〜10質量%) 2.0質量%
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:283)
本実施例の増ちょう剤は以下の化合物の混合物である。
【0088】
【化14】
Figure 0003670361
【0089】
〈台上耐久試験〉
市販#87サイズバーフィールド型ジョイントを用い、所定の高速回転、高トルク条件で、ジョイントが寿命に至るまでの時間を評価した。
【0090】
【比較例1】
硫化油脂及びトリブチルホスファイトを添加せず、同量の鉱油に置き換えた以外は実施例1と同様な組成を有するグリース組成物を実施例1と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0091】
組成
増ちょう剤(実施例1と同様) 17.0質量%
鉱油(126mm2/s@40℃) 80.5質量%
窒化ホウ素粉体(平均粒径:0.7μm) 1.5質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:298)
【0092】
【比較例2】
窒化ホウ素粉体を添加せず、同量の鉱油に置き換えた以外は実施例1と同様な組成を有するグリース組成物を実施例1と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0093】
組成
増ちょう剤(実施例1と同様) 17.0質量%
鉱油(126mm2/s@40℃) 79.0質量%
硫化油脂(硫黄含有量9〜10質量%) 2.0質量%
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:307)
【0094】
【比較例3】
トリブチルホスファイトを添加せず、同量の鉱油に置き換えた以外は実施例1と同様な組成を有するグリース組成物を実施例1と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0095】
組成
増ちょう剤(実施例1と同様) 17.0質量%
鉱油(126mm2/s@40℃) 78.5質量%
窒化ホウ素粉体(平均粒径:0.7μm) 1.5質量%
硫化油脂(硫黄含有量9〜10質量%) 2.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:289)
【0096】
【比較例4】
硫化油脂を添加せず、同量の鉱油に置き換えた以外は実施例1と同様な組成を有するグリース組成物を実施例1と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0097】
組成
増ちょう剤(実施例1と同様) 17.0質量%
鉱油(126mm2/s@40℃) 79.5質量%
窒化ほう素粉体(平均粒径0.7μm) 1.5質量%
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:304)
【0098】
【実施例2】
リチウム−12−ヒドロキシステアレート75gを、550gの鉱油に入れ、攪拌しながら200℃に加熱溶解した後、320gの鉱油を添加して急冷したところゲル状物質を生じた。攪拌を続けながら100℃にて30分間保持した後、添加剤を添加して撹拌し3本ロールミルを通して目的のグリース組成物を調製した。得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0099】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 87.0質量%
窒化ホウ素粉体(平均粒径:0.7μm) 1.5質量%
硫化油脂(硫黄含有量9〜10質量%) 2.0質量%
トリクレジルホスフェート 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:288)
【0100】
【実施例3】
トリクレジルホスフェートを同量のトリブチルホスファイトに置き換えた以外は実施例2と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0101】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 87.0質量%
窒化ホウ素粉体(平均粒径:0.7μm) 1.5質量%
硫化油脂(硫黄含有量9〜10質量%) 2.0質量%
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:286)
【0102】
【実施例4】
硫化油脂を同量のポリサルファイドに置き換えた以外は実施例2と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0103】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 87.0質量%
窒化ホウ素粉体(平均粒径:3μm) 1.5質量%
ジヒドロカルビルポリサルファイド 2.0質量%
(硫黄含有量42質量%)
トリクレジルホスフェート 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:285)
【0104】
【実施例5】
トリクレジルホスフェートを同量のトリブチルホスファイトに、また硫化油脂を同量のポリサルファイドに置き換えた以外は実施例2と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0105】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 87.0質量%
窒化ホウ素粉体(平均粒径:0.7μm) 1.5質量%
ジヒドロカルビルポリサルファイド 2.0質量%
(硫黄含有量42質量%)
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:287)
【0106】
【比較例5】
硫化油脂及びトリクレジルホスフェートを添加せず、同量の鉱油に置き換えた以外は実施例2と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0107】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 90.0質量%
窒化ホウ素粉体(平均粒径:3μm) 1.5質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:298)
【0108】
【比較例6】
窒化ホウ素粉体を添加せず、同量の鉱油に置き換えた以外は実施例5と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0109】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 88.5質量%
ジヒドロカルビルポリサルファイド 2.0質量%
(硫黄含有量42質量%)
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:295)
【0110】
【実施例6】
モリブデンジチオカーバメートを添加した以外は実施例5と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0111】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 84.0質量%
窒化ホウ素粉体(平均粒径:5μm) 1.5質量%
モリブデンジブチルジチオカーバメート 3.0質量%
ジヒドロカルビルポリサルファイド 2.0質量%
(硫黄含有量42質量%)
トリブチルホスファイト 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:292)
【0112】
【実施例7】
モリブデンジチオカーバメートを添加した以外は実施例4と同様な組成を有するグリース組成物を実施例2と同様に調製し、得られたグリース組成物について、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0113】
組成
リチウム−12−ヒドロキシステアレート 7.5質量%
鉱油(126mm2/s@40℃) 84.0質量%
窒化ホウ素粉体(平均粒径:3μm) 1.5質量%
モリブデンジブチルジチオカーバメート 3.0質量%
ジヒドロカルビルポリサルファイド 2.0質量%
(硫黄含有量42質量%)
トリクレジルホスフェート 1.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:290)
【0114】
【実施例8】
ジフェニルメタン−4,4’−ジイソシアネート36.5gを350gの鉱油に入れ、60℃に加熱し、均一に溶解させた。次いでオクタデシルアルコール39.1gを同鉱油250gに加熱溶解させた溶解物を添加し、激しく攪拌した後、さらにシクロヘキシルアミン14.4gを同鉱油195gに溶解させた溶解物を加え、再度激しく攪拌したところ、ゲル状物質が生じた。攪拌を続けながら100℃にて30分間保持した後、添加剤を添加して撹拌し、3本ロールミルを通して目的のグリース組成物を調製した。得られたグリース組成物につき、実施例1と同様な評価試験を行った。結果を表1に示す。またこのグリース組成物の組成を以下に示す。
【0115】
組成
増ちょう剤 9.0質量%
鉱油(126mm2/s@40℃) 79.5質量%
窒化ホウ素粉体(平均粒径:7μm) 1.5質量%
モリブデンジブチルジチオカーバメート 3.0質量%
二硫化モリブデン 2.0質量%
ジヒドロカルビルポリサルファイド 2.0質量%
(硫黄含有量42質量%)
トリブチルホスフェート 2.0質量%
アミン系酸化防止剤 1.0質量%
(混和ちょう度:314)
本実施例の増ちょう剤は以下の化合物の混合物である。
【0116】
【化15】
Figure 0003670361
【0117】
【表1】
Figure 0003670361
【0118】
表1の結果から明らかなように、本発明のグリース組成物は比較例に示すグリース組成物に比較して等速ジョイントの寿命を延長できることがわかる。比較例1、2及び5については焼付き発生により、比較例3、4及び6についてはフレーキングの発生によりジョイント寿命に至っている。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a grease composition for a constant velocity joint which is a fixed joint and a slide joint.
[0002]
[Prior art]
In general, when applying a constant velocity joint in an FF vehicle, a combination of (fixed type joint) + (shaft) + (thrust type joint) is used.
[0003]
Fixed joints include barfield joints, zeppa joints, undercut free joints, tripod joints, and the like, and slide joints include double offset joints, tripod joints, and cross groove joints.
[0004]
As a lubricant used for sealing in these constant velocity joints, an extreme pressure grease has been conventionally used in which molybdenum disulfide, lead compounds, etc. are combined with a base grease consisting of refined mineral oil, lithium soap and urea-based thickener. Mainly used.
[0005]
The constant velocity joint grease is required to have performances such as (1) flaking resistance, (2) seizure resistance, (3) wear resistance, and (4) low friction. However, with the recent trend toward higher performance and higher grades of automobiles, the performance of conventional grease has become insufficient, and there is a strong demand for improved anti-flaking performance, particularly in terms of extending the life of constant velocity joints. .
[0006]
[Problems to be solved by the invention]
An object of the present invention is to provide a grease composition for a constant velocity joint that is particularly excellent in anti-flaking performance and can prolong the life of the constant velocity joint.
[0007]
[Means for Solving the Problems]
  According to the present invention, the base oil is based on the total amount of the composition,
(1) Thickener 2-25% by mass,
(2) boron nitride powder 0.5-20% by mass, and
(3) As an extreme pressure agent, sulfur-phosphorus extreme pressure agent 0.1-10 mass%
And the sulfur-phosphorus extreme pressure agent is
(3-1) A mixture of a sulfur-based extreme pressure agent and a phosphorus-based extreme pressure agent, wherein the sulfur-based extreme pressure agent is a sulfurized oil, sulfur-crosslinked metal phenate, diHydroA sulfur-based extreme pressure agent selected from carbyl polysulfides, dithiocarbamates, monosulfides, sulfoxides, sulfinates and mixtures thereof, wherein the phosphorus-based extreme pressure agent is phosphate, phosphite, phosphinate, phosphonate, amine salts thereof and A mixture which is a phosphorus-based extreme pressure agent selected from these mixturesIsA grease composition for a constant velocity joint is provided.
[0008]
DETAILED DESCRIPTION OF THE INVENTION
Preferred examples of the base oil of the grease composition for constant velocity joints of the present invention include mineral oil and / or synthetic oil. The mineral oil can be obtained by a method commonly used in the manufacturing process of lubricating oil in the petroleum refining industry. For example, a lubricating oil fraction obtained by subjecting crude oil to atmospheric distillation and vacuum distillation can be desolvated and solvent extracted. , Hydrocracking, solvent dewaxing, catalytic dewaxing, hydrorefining, sulfuric acid washing, clay treatment, etc.
[0009]
Specific examples of the synthetic oil include poly α-olefins such as polybutene, 1-octene oligomer, 1-decene oligomer or hydrides thereof; ditridecyl glutarate, di-2-ethylhexyl adipate, diisodecyl adipate, ditri Diesters such as decyl adipate and di-3-ethylhexyl sebacate; polyol esters such as trimethylolpropane caprylate, trimethylolpropane pelargonate, pentaerythritol-2-ethylhexanoate, pentaerythritol pelargonate; alkylnaphthalene; alkylbenzene; Polyoxyalkylene glycols; polyphenyl ethers; dialkyl diphenyl ethers; silicone oils; perfluoroalkyl ethers and the like. Can is used alone or as a mixture.
[0010]
The viscosity range of these base oils can be used as long as it is that of a commonly used lubricating oil, but the kinematic viscosity at 100 ° C. is usually 2 to 40 mm.2/ S, preferably 3-20 mm2/ S is desirable. The base oil preferably has a viscosity index of 90 or more, more preferably 100 or more.
[0011]
The grease composition for constant velocity joints of the present invention contains a thickener as an essential component. As the thickener, various thickeners such as soaps such as metal soaps and composite metal soaps; non-soaps such as benton, silica gel, urea compounds, urea / urethane compounds and urethane compounds can be used. From the viewpoint of properties, a urea compound, a urea / urethane compound, a urethane compound, or a mixture thereof is preferable.
[0012]
Examples of the soap-based thickener include sodium soap, calcium soap, aluminum soap, lithium soap and the like.
[0013]
Examples of the urea compound, urea / urethane compound, and urethane compound include diurea compounds, triurea compounds, tetraurea compounds, other polyurea compounds, urea / urethane compounds, diurethane compounds, and mixtures thereof. More preferably, the diurea compound, the urea-urethane compound, the diurethane compound or a mixture thereof can be mentioned, and more specifically, for example, the compound represented by the following general formula (1) alone or a mixture thereof is preferable. .
[0014]
[Chemical 1]
Figure 0003670361
[0015]
R in the general formula (1)1Is preferably a divalent hydrocarbon group having 6 to 20 carbon atoms, particularly preferably 6 to 15 carbon atoms. Examples of the divalent hydrocarbon group include a linear or branched alkylene group, a linear or branched alkenylene group, a cycloalkylene group, and an aromatic group. R1Specific examples thereof include an ethylene group, 2,2-dimethyl-4-methylhexylene group, and groups represented by the following formulas (a) to (j).
[0016]
[Chemical 2]
Figure 0003670361
[0017]
[Chemical 3]
Figure 0003670361
[0018]
Among these, (d) and (e) are particularly preferable.
[0019]
R in the general formula (1)2, RThree, RFourAnd RFiveExamples of the alkyl group include a linear or branched alkyl group, a linear or branched alkenyl group, a cycloalkyl group, an alkylcycloalkyl group, an aryl group, an alkylaryl group, and an arylalkyl group. Specifically, for example, hexyl group, heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group, nonadecyl group, eicosyl group Linear or branched alkyl groups such as hexenyl, heptenyl, octenyl, nonenyl, decenyl, undecenyl, dodecenyl, tridecenyl, tetradecenyl, pentadecenyl, hexadecenyl, heptadecenyl, octadecenyl, nonadecenyl Group, straight chain or branched alkenyl group such as eicosenyl group; cyclohexyl group; methylcyclohexyl group, dimethylcyclohexyl group, ethylcyclohexyl group, diethylcyclohexyl group, propylcyclohexyl group, isopropyl Cyclohexyl group, 1-methyl-3-propylcyclohexyl group, butylcyclohexyl group, amylcyclohexyl group, amylmethylcyclohexyl group, hexylcyclohexyl group, heptylcyclohexyl group, octylcyclohexyl group, nonylcyclohexyl group, decylcyclohexyl group, undecylcyclohexyl group Alkylcycloalkyl groups such as dodecylcyclohexyl group, tridecylcyclohexyl group and tetradecylcyclohexyl group; aryl groups such as phenyl group and naphthyl group; toluyl group, ethylphenyl group, xylyl group, propylphenyl group, cumenyl group, methylnaphthyl group Group, ethyl naphthyl group, dimethyl naphthyl group, propyl naphthyl group and other alkylaryl groups; benzyl group, methylbenzyl group, ethylbenzyl group Ruarukiru group can be exemplified, and among these the cyclohexyl group, octadecyl group and toluyl group are particularly preferred.
[0020]
To produce the diurea compound, urea-urethane compound or diurethane compound, for example, the general formula OCN-R1A diisocyanate represented by -NCO and a general formula R2NH2, RThreeRFourNH or RFiveIt can be obtained by reacting a compound represented by OH or a mixture thereof in a base oil at 10 to 200 ° C. At this time R1, R2, RThree, RFourAnd RFiveIs R in the general formula (1)1, R2, RThree, RFourAnd RFiveIs the same.
[0021]
The content of the thickener is 2 to 25% by mass, preferably 3 to 20% by mass, based on the total amount of the grease composition. When the content of the thickener is less than 2% by mass, the effect as a thickener is small, so that it does not become a sufficient grease, and when it exceeds 25% by mass, it becomes too hard as a grease and sufficient lubrication performance is obtained. I can't demonstrate it.
[0022]
The grease composition of the present invention contains boron nitride powder as an essential component. The particle size of the boron nitride powder is not particularly limited, but the average particle size is usually 0.05 to 20 μm, preferably 0.4 to 15 μm, more preferably 5 to 10 μm.
[0023]
The content of the boron nitride powder is 0.5 to 20% by mass, preferably 1 to 20% by mass, based on the total amount of the grease composition. When the content of the boron nitride powder is less than 0.5% by mass, the anti-flaking performance is hindered, and the seizure life of the constant velocity joint is insufficient. On the other hand, when the content of the boron nitride powder exceeds 20% by mass, rough wear (wear due to the grinding action of the particles) is promoted, and the life of the constant velocity joint becomes insufficient.
[0024]
The grease composition of the present invention contains a sulfur-phosphorus extreme pressure agent as an essential component.
[0025]
  The sulfur-phosphorus extreme pressure agent andThe sulfurSulfur extreme pressure agent containing only yellow and phosphorus extreme pressure agent containing only phosphorusIt is a mixture of
[0026]
The ratio of sulfur atoms to phosphorus atoms in the sulfur-phosphorus extreme pressure agent is preferably in the range of 100: 25 to 100: 1.
[0027]
  The sulfur-based extreme pressure agent andThe sulfurOils and fats, sulfur cross-linked metal phenates, dihydrocarbyl polysulfides, dithiocarbamates, monosulfides, sulfoxides, sulfinatesAnd a sulfur-based extreme pressure agent selected from these mixtures. ThisAmong these, sulfurized fats and oils, dihydrocarbyl polysulfide, or a mixture thereof is preferable.
[0028]
The sulfurized fats and oils include olive oil, castor oil, tea seed oil, nutka oil, cottonseed oil, rapeseed oil, corn oil, beef tallow, cow leg oil, sperm whale oil, whale wax, etc. , Refers to a compound obtained by heating. The sulfur content of the sulfurized fat / oil is usually 5 to 15% by mass, preferably 8 to 12% by mass.
[0029]
Examples of the sulfur-crosslinked metal phenate include an alkaline earth metal salt of an alkylphenol sulfide to which an alkyl group having 8 to 30 carbon atoms, preferably 9 to 20 carbon atoms, is added. Specific examples of the alkyl group include octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, nonadecyl, icosyl, heicosyl, A docosyl group, a tricosyl group, a tetracosyl group, a pentacosyl group, a hexacosyl group, a heptacosyl group, an octacosyl group, a nonacosyl group, a triacontyl group, etc. are mentioned, These may be linear or branched. The alkyl group is preferably derived from nonene, an olefin having 5 to 8 carbon atoms or an alcohol. The alkaline earth metal is preferably magnesium, calcium or barium.
[0030]
The dihydrocarbyl polysulfide means a compound represented by the following general formula (2).
[0031]
[Formula 4]
Figure 0003670361
[0032]
Where R6And R7Are the same or different groups and are alkyl groups derived from propylene or isobutene having 3 to 18, preferably 6 to 15 carbon atoms, or aryl groups, alkylaryl groups or arylalkyl groups having 6 to 8 carbon atoms. Preferably, these groups include, for example, an isopropyl group, a branched hexyl group derived from a propylene dimer, a branched nonyl group derived from a propylene trimer, and a branch derived from a propylene tetramer. Dodecyl group, branched pentadecyl group derived from propylene pentamer, branched octadecyl group derived from propylene hexamer, tert-butyl group, branched octyl group derived from isobutene dimer, isobutene trimer Alkyl groups such as branched dodecyl groups derived from the body and branched hexadecyl groups derived from the isobutene tetramer These alkyl groups include all branched isomers.); Alkylaryl groups such as phenyl group, tolyl group, ethylphenyl group, xylyl group (the alkyl part of these alkylaryl groups may be linear or branched, The substitution position on the aryl group of the alkyl moiety is arbitrary.); Or arylalkyl groups such as a benzyl group and a phenylethyl group (the substitution position of the phenyl group is arbitrary).
[0033]
Z in General formula (2) shows the number of 1-5, Preferably 2-4. When z is 3 or more,
[0034]
[Chemical formula 5]
Figure 0003670361
[0035]
A ring may be formed as shown below.
[0036]
Specific examples of the dihydrocarbyl polysulfide include dibutyl polysulfide, dihexyl polysulfide, dioctyl polysulfide, dinonyl polysulfide, didecyl polysulfide, didodecyl polysulfide, ditetradecyl polysulfide, dihexadecyl polysulfide, dioctadecyl polysulfide, dieicosyl polysulfide, Examples thereof include diphenyl polysulfide, dibenzyl polysulfide, diphenethyl polysulfide, polypropenyl polysulfide, polybutenyl polysulfide, and a mixture thereof. Polypropenyl polysulfide, polybutenyl polysulfide, and a mixture thereof are particularly preferable.
[0037]
The polypropenyl polysulfide, polybutenyl polysulfide, or a mixture thereof includes propylene, isobutene, a dimer to tetramer of these monomers, or an olefinic hydrocarbon such as a mixture of these monomers or polymers, elemental sulfur, It can be obtained by sulfurization with a halogenated sulfur (for example, sulfur monochloride or sulfur dichloride), hydrogen sulfide or a mixture thereof.
[0038]
The sulfur content of the dihydrocarbyl polysulfide is usually 30 to 50% by mass, preferably 40 to 45% by mass.
[0039]
Examples of the dithiocarbamates include alkylthiocarbamyl compounds represented by the following general formula (3).
[0040]
[Chemical 6]
Figure 0003670361
[0041]
Where R8, R9, RTenAnd R11Are the same or different groups, and each represents a linear or branched alkyl group having 1 to 18 carbon atoms, preferably 1 to 10 carbon atoms, specifically, a methyl group, an ethyl group, a propyl group, an n-butyl group. And alkyl groups such as isobutyl, pentyl, isopentyl, hexyl, heptyl, octyl, 2-ethylhexyl, nonyl, decyl, tridecyl or octadecyl.
[0042]
In the formula, (Y) is S, S-S, S-CH.2-S, S- (CH2)2-S, S- (CH2)Three-S or S-Zn-S is represented.
[0043]
Specific examples of the alkyldithiocarbamyl compound include methylenebis (dibutyldithiocarbamate), bis (dimethylthiocarbamyl) monosulfide, bis (dimethylthiocarbamyl) disulfide, bis (dibutylthiocarbamyl) disulfide, bis (Dipentylthiocarbamyl) disulfide, bis (dioctylthiocarbamyl) disulfide, zinc dipentyl dithiocarbamate and the like can be mentioned.
[0044]
  The phosphorus-based extreme pressure agent andIs hoSulfate, phosphite, phosphinate, phosphonateGThese amine saltsAnd a phosphorus-based extreme pressure agent selected from a mixture thereof.Among these, phosphate, phosphite or a mixture thereof is preferable.
[0045]
The phosphate here refers to a compound represented by the following general formula (4), and the phosphite refers to a compound represented by the following general formula (5).
[0046]
[Chemical 7]
Figure 0003670361
[0047]
[Chemical 8]
Figure 0003670361
[0048]
Where R12Represents an alkyl group having 1 to 24 carbon atoms, a cycloalkyl group, an alkylcycloalkyl group, an alkenyl group, an aryl group, an alkylaryl group, an arylalkyl group, or the like;13And R14Represents a hydrogen atom, an alkyl group having 1 to 24 carbon atoms, a cycloalkyl group, an alkylcycloalkyl group, an alkenyl group, an aryl group, an alkylaryl group, an arylalkyl group, or the like.
[0049]
R12, R13And R14Specific examples other than the hydrogen atom include methyl group, ethyl group, propyl group, butyl group, pentyl group, hexyl group, heptyl group, octyl group, nonyl group, decyl group, dodecyl group, tetradecyl group, hexadecyl group, octadecyl group , Eicosyl group, docosyl group, tetracosyl group, cyclopentyl group, cyclohexyl group, methylcyclohexyl group, ethylcyclohexyl group, dimethylcyclohexyl group, cycloheptyl group, phenyl group, tolyl group, xylyl group, ethylphenyl group, propylphenyl group, butyl Examples include phenyl, pentylphenyl, hexylphenyl, nonylphenyl, decylphenyl, dodecylphenyl, tetradecylphenyl, hexadecylphenyl, octadecylphenyl, benzyl or phenethyl. Can.
[0050]
Specific examples of the phosphorous extreme pressure agent include tributyl phosphate, benzyl diphenyl phosphate, ethyl diphenyl phosphate, octyl diphenyl phosphate, triphenyl phosphate, tricresyl phosphate, tolyl phosphate, 2-ethylhexyl diphenyl phosphate, tributyl phosphate, dibutyl phosphate And lauryl phosphite.
[0051]
The combined use of the sulfur-based extreme pressure agent and the phosphorus-based extreme pressure agent is particularly preferably the combined use of the dihydrocarbyl polysulfide and the phosphate, or the combined use of the sulfurized oil and fat and the phosphate.
[0053]
The content of the sulfur-phosphorus extreme pressure agent in the grease composition of the present invention is 0.1 to 10% by mass, preferably 1 to 5% by mass, based on the total amount of the grease composition. When the content of the sulfur-phosphorus extreme pressure agent is less than 0.1% by mass, the seizure life of the constant velocity joint becomes insufficient. On the other hand, if the content of the sulfur-phosphorus extreme pressure agent exceeds 10% by mass, the performance corresponding to the addition amount cannot be obtained, which is uneconomical.
[0054]
The grease composition for constant velocity joints of the present invention can further contain molybdenum dithiocarbamate as an extreme pressure agent in addition to the sulfur-phosphorus extreme pressure agent.
[0055]
Examples of the molybdenum dithiocarbamate include those represented by the following general formula (6).
[0056]
[Chemical 9]
Figure 0003670361
[0057]
Where R15, R16, R17And R18Are the same or different groups and each represents a hydrocarbon group such as an alkyl group, an alkenyl group, an aryl group, an alkylaryl group, or an arylalkyl group, with an alkyl group being particularly preferred.
[0058]
R15, R16, R17And R18Specific examples of the ethyl group, propyl group, butyl group, pentyl group, hexyl group, heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, Examples thereof include linear or branched alkyl groups having 2 to 18 carbon atoms such as heptadecyl group and octadecyl group, preferably 8 to 13; alkylaryl groups such as butylphenyl group and nonylphenyl group. X1, X2, XThreeAnd XFourEach represents a sulfur atom or an oxygen atom.
[0059]
Specific examples of the molybdenum dithiocarbamate include molybdenum sulfide diethyldithiocarbamate, molybdenum dipropyldithiocarbamate, molybdenum dibutyldithiocarbamate, molybdenum dipentyldithiocarbamate, molybdenum dihexyldithiocarbamate, molybdenum dioctyldithiocarbamate, molybdenum dioctyldithiocarbamate, and molybdenum didecyldithiocarbamate. , Molybdenum sulfide didodecyl dithiocarbamate, Molybdenum ditridecyl dithiocarbamate, Molybdenum di (butylphenyl) dithiocarbamate, Molybdenum di (nonylphenyl) dithiocarbamate, Oxymolybdenum diethyldithiocarbamate, Oxymolybdenum dipropyldithiocarbamate, Oxymolybdenum sulfide Butyl dithiocarbamate, sulfurized oxymolybdenum dipentyldithiocarbamate, sulfurized oxymolybdenum dihexyldithiocarbamate, sulfurized oxymolybdenum dioctyldithiocarbamate, sulfurized oxymolybdenum didecyldithiocarbamate, sulfurized oxymolybdenum didodecyldithiocarbamate, sulfurized oxymolybdenum ditridecyldithiocarbamate, sulfurized oxymolybdenum disulfide (Butylphenyl) dithiocarbamate, sulfurized oxymolybdenum di (nonylphenyl) dithiocarbamate and the like can be mentioned. Each of these compounds can be used alone or as a mixture.
[0060]
The content of the molybdenum dithiocarbamate in the grease composition of the present invention is usually 0.1 to 10% by mass, preferably 1 to 5% by mass, based on the total amount of the grease composition.
[0061]
The weight ratio when the molybdenum dithiocarbamate and the sulfur-phosphorus extreme pressure agent are used in combination is usually from molybdenum dithiocarbamate: sulfur-phosphorus extreme pressure agent to 1: 5 to 5: 1, preferably 1: 3. 3: 1 is desirable.
[0062]
Moreover, anti-flake performance can be further improved by adding an organic zinc compound to the grease composition of the present invention. Examples of the organic zinc compound include zinc dithiophosphate, zinc dithiocarbamate, fatty acid zinc salt, and zinc naphthenate.
[0063]
Examples of the zinc dithiophosphate include compounds represented by the following general formula (7).
[0064]
[Chemical Formula 10]
Figure 0003670361
[0065]
Where R19, R20, Rtwenty oneAnd Rtwenty twoAre the same or different groups, and each represents a linear or branched primary or secondary alkyl group, aryl group or arylalkyl group having 2 to 18 carbon atoms, specifically, ethyl group, propyl group, butyl group Group, pentyl group, hexyl group, heptyl group, octyl group, nonyl group, decyl group, undecyl group, dodecyl group, tridecyl group, tetradecyl group, pentadecyl group, hexadecyl group, heptadecyl group, octadecyl group and the like.
[0066]
Moreover, as said zinc dithiocarbamate, the compound represented by following General formula (8) is mentioned.
[0067]
Embedded image
Figure 0003670361
[0068]
Where Rtwenty three, Rtwenty four, Rtwenty fiveAnd R26Are the same or different groups and each represents an alkyl group, alkenyl group, aryl group, alkylaryl group or arylalkyl group having 2 to 18 carbon atoms, specifically an ethyl group, a propyl group, a butyl group, a pentyl group. Alkyl groups such as hexyl, heptyl, octyl, nonyl, decyl, undecyl, dodecyl, tridecyl, tetradecyl, pentadecyl, hexadecyl, heptadecyl, octadecyl, etc. Or may be branched, and may be primary or secondary.); Alkylaryl groups such as butylphenyl group and nonylphenyl group (the alkyl part of these alkylaryl groups may be linear or branched, and the aryl of the alkyl part) The substitution position on the group is arbitrary.
[0069]
Examples of the fatty acid zinc salt include compounds represented by the following general formula (9).
[0070]
Embedded image
Figure 0003670361
[0071]
Where R27Represents an alkyl group or an alkenyl group having 3 to 22 carbon atoms.
[0072]
Examples of the naphthenic acid zinc salt include compounds represented by the following general formula (10).
[0073]
Embedded image
Figure 0003670361
[0074]
Where R28Represents a cycloalkyl group such as a cyclopentyl group, a cyclohexyl group, an alkylcyclopentyl group, an alkylcyclohexyl group, and m represents an integer.
[0075]
When the organozinc compound is contained in the grease composition of the present invention, the content is usually 0.1 to 10% by mass, preferably 1 to 5% by mass, based on the total amount of the grease composition.
[0076]
In addition, in the grease composition for constant velocity joints of the present invention, as long as the properties thereof are not impaired, a solid lubricant; other than the sulfur-phosphorus system and molybdenum dithiocarbamate as required, in order to further improve the performance. Other additives such as extreme pressure agents; antioxidants; oiliness agents; rust inhibitors; viscosity index improvers can be included.
[0077]
Specific examples of the solid lubricant include graphite, graphite fluoride, polytetrafluoroethylene, molybdenum disulfide, antimony sulfide, and alkali (earth) metal borate.
[0078]
Specific examples of the other extreme pressure agent include chlorine compounds such as chlorinated paraffin and chlorinated ester; molybdenum compounds such as molybdenum dithiophosphate.
[0079]
Specific examples of the antioxidant include phenol compounds such as 2,6-di-t-butylphenol and 2,6-di-t-butyl-p-cresol, dialkyldiphenylamine, phenyl-α-naphthylamine, p. Examples include amine compounds such as -alkylphenyl-α-naphthylamine, sulfur compounds, and phenothiazine compounds.
[0080]
Specific examples of the oily agent include amines such as laurylamine, myristylamine, palmitylamine, stearylamine and oleylamine; higher alcohols such as lauryl alcohol, myristyl alcohol, palmityl alcohol, stearyl alcohol and oleyl alcohol; Higher fatty acids such as acid, myristic acid, palmitic acid, stearic acid, oleic acid; fatty acid esters such as methyl laurate, methyl myristate, methyl palmitate, methyl stearate, methyl oleate; laurylamide, myristylamide, palmityl Amides such as amide, stearylamide and oleylamide;
[0081]
Specific examples of the rust inhibitor include metal soaps; synthetic sulfonates such as petroleum sulfonates, alkylbenzene sulfonates and dinonylnaphthalene sulfonates; polyhydric alcohol partial esters such as sorbitan fatty acid esters; amines; phosphoric acid; Can be mentioned.
[0082]
Specific examples of the viscosity index improver include polymethacrylate, polyisobutylene, polystyrene and the like.
[0083]
To prepare the grease composition for constant velocity joints of the present invention, for example, the base oil, the thickener, the boron nitride powder, the sulfur-phosphorus extreme pressure agent, and if necessary, the molybdenum dithiol. It can be obtained by stirring the carbamate, the organozinc compound or the other additive and passing it through a roll mill or the like. In addition, a thickener raw material component is added to the base oil in advance, melted, and stirred and mixed to prepare the thickener, and at the same time, the grease composition of the present invention can be produced.
[0084]
【The invention's effect】
The grease composition for constant velocity joints of the present invention has excellent anti-flaking performance and can extend the life of the constant velocity joint.
[0085]
【Example】
Hereinafter, the content of the present invention will be described more specifically with reference to Examples and Comparative Examples, but the present invention is not limited thereto.
[0086]
[Example 1]
Diphenylmethane-4,4'-diisocyanate (88.0 g) was placed in 350 g of mineral oil, heated to 60 ° C, and uniformly dissolved. Next, a solution in which 26.2 g of dodecyl alcohol was dissolved by heating in 200 g of the same mineral oil was added and stirred vigorously, and then a solution in which 55.8 g of cyclohexylamine was dissolved in 205 g of the same mineral oil was added and stirred vigorously again. A gel-like substance was produced. After maintaining at 100 ° C. for 30 minutes while continuing the stirring, an additive containing a thickener, boron nitride powder and an extreme pressure agent was added and stirred, and the desired grease composition was prepared through a three-roll mill. The obtained grease composition was evaluated by the following method. The results are shown in Table 1. The composition of this grease composition is shown below.
[0087]
composition
Thickener 17.0% by mass
Mineral oil (126mm2/ S @ 40 ° C) 77.5 mass%
Boron nitride powder (average particle size: 0.7 μm) 1.5% by mass
Sulfurized fat (sulfur content 9-10% by mass) 2.0% by mass
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 283)
The thickener of this example is a mixture of the following compounds:
[0088]
Embedded image
Figure 0003670361
[0089]
<Bench durability test>
A commercially available # 87 size barfield type joint was used, and the time until the joint reached the end of its service life was evaluated under predetermined high-speed rotation and high torque conditions.
[0090]
[Comparative Example 1]
A grease composition having the same composition as in Example 1 was prepared in the same manner as in Example 1 except that sulfur oil and fat and tributyl phosphite were not added and replaced with the same amount of mineral oil. The same evaluation test as in Example 1 was performed. The results are shown in Table 1. The composition of this grease composition is shown below.
[0091]
composition
Thickener (same as Example 1) 17.0% by mass
Mineral oil (126mm2/ S @ 40 ° C) 80.5 mass%
Boron nitride powder (average particle size: 0.7 μm) 1.5% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 298)
[0092]
[Comparative Example 2]
A grease composition having the same composition as in Example 1 was prepared in the same manner as in Example 1 except that the boron nitride powder was not added and replaced with the same amount of mineral oil. The same evaluation test as 1 was performed. The results are shown in Table 1. The composition of this grease composition is shown below.
[0093]
composition
Thickener (same as Example 1) 17.0% by mass
Mineral oil (126mm2/ S @ 40 ° C) 79.0% by mass
Sulfurized fat (sulfur content 9-10% by mass) 2.0% by mass
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 307)
[0094]
[Comparative Example 3]
A grease composition having the same composition as in Example 1 was prepared in the same manner as in Example 1 except that tributyl phosphite was not added and replaced with the same amount of mineral oil. The same evaluation test was conducted. The results are shown in Table 1. The composition of this grease composition is shown below.
[0095]
composition
Thickener (same as Example 1) 17.0% by mass
Mineral oil (126mm2/ S @ 40 ° C) 78.5% by mass
Boron nitride powder (average particle size: 0.7 μm) 1.5% by mass
Sulfurized fat (sulfur content 9-10% by mass) 2.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 289)
[0096]
[Comparative Example 4]
A grease composition having the same composition as in Example 1 was prepared in the same manner as in Example 1 except that the same amount of mineral oil was replaced without adding sulfurized fats and oils. A similar evaluation test was conducted. The results are shown in Table 1. The composition of this grease composition is shown below.
[0097]
composition
Thickener (same as Example 1) 17.0% by mass
Mineral oil (126mm2/ S @ 40 ° C) 79.5 mass%
Boron nitride powder (average particle size 0.7μm) 1.5% by mass
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 304)
[0098]
[Example 2]
75 g of lithium-12-hydroxystearate was put into 550 g of mineral oil, heated and dissolved at 200 ° C. with stirring, and then 320 g of mineral oil was added and quenched to produce a gel substance. While maintaining stirring at 100 ° C. for 30 minutes, the additive was added and stirred, and the desired grease composition was prepared through a three-roll mill. The obtained grease composition was subjected to the same evaluation test as in Example 1. The results are shown in Table 1. The composition of this grease composition is shown below.
[0099]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 87.0 mass%
Boron nitride powder (average particle size: 0.7 μm) 1.5% by mass
Sulfurized fat (sulfur content 9-10% by mass) 2.0% by mass
Tricresyl phosphate 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 288)
[0100]
[Example 3]
A grease composition having the same composition as in Example 2 except that tricresyl phosphate was replaced with the same amount of tributyl phosphite was prepared in the same manner as in Example 2. The resulting grease composition was A similar evaluation test was conducted. The results are shown in Table 1. The composition of this grease composition is shown below.
[0101]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 87.0 mass%
Boron nitride powder (average particle size: 0.7 μm) 1.5% by mass
Sulfurized oil (sulfur content 9-10% by mass) 2.0% by mass
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 286)
[0102]
[Example 4]
A grease composition having the same composition as in Example 2 was prepared except that the sulfurized fat was replaced with the same amount of polysulfide. The grease composition thus obtained was evaluated in the same manner as in Example 1. Went. The results are shown in Table 1. The composition of this grease composition is shown below.
[0103]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 87.0 mass%
Boron nitride powder (average particle size: 3 μm) 1.5% by mass
Dihydrocarbyl polysulfide 2.0% by mass
(Sulfur content 42% by mass)
Tricresyl phosphate 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 285)
[0104]
[Example 5]
A grease composition having the same composition as in Example 2 except that tricresyl phosphate was replaced with the same amount of tributyl phosphite and sulfurized fat and oil was replaced with the same amount of polysulfide was prepared in the same manner as in Example 2. The grease composition was subjected to the same evaluation test as in Example 1. The results are shown in Table 1. The composition of this grease composition is shown below.
[0105]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 87.0 mass%
Boron nitride powder (average particle size: 0.7 μm) 1.5% by mass
Dihydrocarbyl polysulfide 2.0% by mass
(Sulfur content 42% by mass)
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 287)
[0106]
[Comparative Example 5]
A grease composition having the same composition as in Example 2 was prepared in the same manner as in Example 2 except that sulfur oil and fat and tricresyl phosphate were not added and replaced with the same amount of mineral oil. The same evaluation test as in Example 1 was performed. The results are shown in Table 1. The composition of this grease composition is shown below.
[0107]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 90.0 mass%
Boron nitride powder (average particle size: 3 μm) 1.5% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 298)
[0108]
[Comparative Example 6]
A grease composition having the same composition as in Example 5 was prepared in the same manner as in Example 2 except that the boron nitride powder was not added and replaced with the same amount of mineral oil. The same evaluation test as 1 was performed. The results are shown in Table 1. The composition of this grease composition is shown below.
[0109]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 88.5 mass%
Dihydrocarbyl polysulfide 2.0% by mass
(Sulfur content 42% by mass)
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 295)
[0110]
[Example 6]
A grease composition having the same composition as in Example 5 except that molybdenum dithiocarbamate was added was prepared in the same manner as in Example 2, and the obtained grease composition was subjected to the same evaluation test as in Example 1. The results are shown in Table 1. The composition of this grease composition is shown below.
[0111]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 84.0% by mass
Boron nitride powder (average particle size: 5 μm) 1.5% by mass
Molybdenum dibutyldithiocarbamate 3.0% by mass
Dihydrocarbyl polysulfide 2.0% by mass
(Sulfur content 42% by mass)
Tributyl phosphite 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 292)
[0112]
[Example 7]
A grease composition having the same composition as in Example 4 except that molybdenum dithiocarbamate was added was prepared in the same manner as in Example 2, and the obtained grease composition was subjected to the same evaluation test as in Example 1. The results are shown in Table 1. The composition of this grease composition is shown below.
[0113]
composition
Lithium-12-hydroxystearate 7.5% by mass
Mineral oil (126mm2/ S @ 40 ° C) 84.0% by mass
Boron nitride powder (average particle size: 3 μm) 1.5% by mass
Molybdenum dibutyldithiocarbamate 3.0% by mass
Dihydrocarbyl polysulfide 2.0% by mass
(Sulfur content 42% by mass)
Tricresyl phosphate 1.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 290)
[0114]
[Example 8]
36.5 g of diphenylmethane-4,4'-diisocyanate was placed in 350 g of mineral oil and heated to 60 ° C. to dissolve it uniformly. Next, a solution in which 39.1 g of octadecyl alcohol was dissolved by heating in 250 g of the same mineral oil was added and stirred vigorously, and then a solution in which 14.4 g of cyclohexylamine was dissolved in 195 g of the same mineral oil was added and vigorously stirred again. A gel-like substance was produced. While maintaining stirring at 100 ° C. for 30 minutes, the additive was added and stirred, and the desired grease composition was prepared through a three-roll mill. The obtained grease composition was subjected to the same evaluation test as in Example 1. The results are shown in Table 1. The composition of this grease composition is shown below.
[0115]
composition
Thickener 9.0% by mass
Mineral oil (126mm2/ S @ 40 ° C) 79.5 mass%
Boron nitride powder (average particle size: 7 μm) 1.5% by mass
Molybdenum dibutyldithiocarbamate 3.0% by mass
Molybdenum disulfide 2.0% by mass
Dihydrocarbyl polysulfide 2.0% by mass
(Sulfur content 42% by mass)
Tributyl phosphate 2.0% by mass
Amine antioxidant 1.0% by mass
(Mixture penetration: 314)
The thickener of this example is a mixture of the following compounds:
[0116]
Embedded image
Figure 0003670361
[0117]
[Table 1]
Figure 0003670361
[0118]
As is apparent from the results in Table 1, it can be seen that the grease composition of the present invention can extend the life of the constant velocity joint as compared with the grease composition shown in the comparative example. In Comparative Examples 1, 2, and 5, the joint life is reached due to seizure occurrence, and in Comparative Examples 3, 4 and 6, flaking occurs.

Claims (2)

基油に、組成物全量を基準として、
(1)増ちょう剤2〜25質量%、
(2)窒化ホウ素粉体0.5〜20質量%、及び
(3)極圧剤として、硫黄−リン系極圧剤0.1〜10質量%
を含有し、前記硫黄−リン系極圧剤が
(3−1)硫黄系極圧剤及びリン系極圧剤の混合物であって、前記硫黄系極圧剤が硫化油脂、硫黄架橋された金属フェネート、ジヒドロカルビルポリサルファイド、ジチオカーバメート類、モノスルフィド、スルホキシド、スルフィネート及びこれらの混合物から選ばれる硫黄系極圧剤であり、前記リン系極圧剤がホスフェート、ホスファイト、ホスフィネート、ホスホネート、これらのアミン塩及びこれらの混合物の中から選ばれるリン系極圧剤である混合物であることを特徴とする等速ジョイント用グリース組成物。
In the base oil, based on the total amount of the composition,
(1) Thickener 2-25% by mass,
(2) Boron nitride powder 0.5 to 20% by mass, and (3) Sulfur-phosphorus extreme pressure agent 0.1 to 10% by mass as the extreme pressure agent
The sulfur-phosphorus extreme pressure agent is (3-1) a mixture of a sulfur extreme pressure agent and a phosphorus extreme pressure agent, and the sulfur extreme pressure agent is a sulfurized oil or fat, sulfur-crosslinked metal phenates, di hydrocarbyl polysulfides, dithiocarbamates, monosulfide, sulfoxide, sulfur-based extreme pressure additive selected from sulfinate and mixtures thereof, said phosphorus-based extreme pressure agent is a phosphate, phosphite, phosphinate, phosphonate, these amine salts of and a constant velocity joint grease composition characterized mixture Dearuko and a phosphorus extreme pressure agent selected from among mixtures thereof.
極圧剤として、さらにモリブデンジチオカーバメートを含有することを特徴とする請求項1記載の等速ジョイント用グリース組成物。  The grease composition for constant velocity joints according to claim 1, further comprising molybdenum dithiocarbamate as an extreme pressure agent.
JP25898295A 1995-10-05 1995-10-05 Grease composition for constant velocity joints Expired - Lifetime JP3670361B2 (en)

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JP3808609B2 (en) * 1997-10-21 2006-08-16 新日本石油株式会社 Grease composition for rolling bearings
JP4004276B2 (en) * 2001-11-21 2007-11-07 株式会社松村石油研究所 Grease composition
JP2005008744A (en) * 2003-06-18 2005-01-13 Showa Shell Sekiyu Kk Grease composition
JP5022582B2 (en) * 2005-08-24 2012-09-12 Ntn株式会社 Grease composition for constant velocity joints
US20070161518A1 (en) * 2006-01-11 2007-07-12 National Starch And Chemical Investment Holding Corporation Boron Nitride Based Lubricant Additive
BRPI0917016A2 (en) * 2008-08-11 2016-02-16 Shell Int Research lubricant composition and use of a lubricant composition
JP4877343B2 (en) * 2009-03-05 2012-02-15 日本精工株式会社 Rolling bearing
JP5113807B2 (en) * 2009-06-19 2013-01-09 昭和シェル石油株式会社 Grease composition for constant velocity joints
JP5665298B2 (en) * 2009-10-05 2015-02-04 協同油脂株式会社 Grease composition and constant velocity joint
JP6292569B2 (en) 2013-12-04 2018-03-14 協同油脂株式会社 Grease composition for constant velocity joint and constant velocity joint enclosing the grease composition
CN108003063B (en) * 2016-10-27 2020-05-19 中国石油化工股份有限公司 Compound and lubricating grease with antioxidant and thickening functions and preparation method thereof
CN108003066B (en) * 2016-10-27 2020-06-12 中国石油化工股份有限公司 Compound with thickening effect, lubricating grease and preparation method thereof
CN107986992B (en) * 2016-10-27 2020-06-16 中国石油化工股份有限公司 Compound with thickening effect, lubricating grease and preparation method thereof
CN108003064B (en) * 2016-10-27 2020-06-16 中国石油化工股份有限公司 Compound with thickening effect, lubricating grease and preparation method thereof
CN107986993B (en) * 2016-10-27 2020-06-16 中国石油化工股份有限公司 Compound with thickening effect, lubricating grease and preparation method thereof

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JPS6346299A (en) * 1986-01-16 1988-02-27 Ntn Toyo Bearing Co Ltd Grease for constant speed joint
JP2799634B2 (en) * 1991-03-07 1998-09-21 日本石油株式会社 Grease composition for constant velocity joints
JP2989311B2 (en) * 1991-04-30 1999-12-13 協同油脂株式会社 Grease composition for constant velocity joints
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