CN111139117B - 含有防剥落剂的润滑剂组合物 - Google Patents

含有防剥落剂的润滑剂组合物 Download PDF

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CN111139117B
CN111139117B CN201911072031.7A CN201911072031A CN111139117B CN 111139117 B CN111139117 B CN 111139117B CN 201911072031 A CN201911072031 A CN 201911072031A CN 111139117 B CN111139117 B CN 111139117B
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compound
glycol
mass
dimethyl
group
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CN111139117A (zh
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纳山慧之
羽山诚
董大明
中山景次
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Kyodo Yushi Co Ltd
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Abstract

本发明提供一种防剥落剂和含有其的润滑剂组合物，所述防剥落剂含有以防剥落剂的总质量为基准超过1质量％的量的、选自(A)体积固有电阻率为1.0×1010Ω·cm以下的化合物和(B)构成分子的全部碳原子中形成芳香环结构的碳原子数的比例为50％以上的化合物中的至少1种。

Description

含有防剥落剂的润滑剂组合物
技术领域
本发明涉及在能够应用于滚动轴承等的金属表面的润滑剂中可以含有的新的防剥落剂。本发明还涉及含有前述防剥落剂的润滑剂组合物。
背景技术
伴随着在滚动轴承的滚动面上产生的白色组织变化而产生的特异性早期异常剥落，会使滚动轴承的疲劳寿命降低，因此，从1980年代中期开始着就成为了问题。这样的剥落被称为白色剥落、白相剥落、脆性剥落、氢脆性剥落或氢脆化剥落等。
这样的剥落产生的机制尚不明确，但例如在专利文献1中介绍了氢学说。即，如果在高负荷下使用润滑脂，则润滑脂分解而产生氢。该氢侵入滚动轴承的钢材内部，在晶界与硬质合金发生反应。其结果是，有时钢材会变脆。专利文献1中报告，通过在润滑脂组合物中含有称为噻唑衍生物、硫化润滑脂或硫化烯烃的、至少含有1个硫原子的特定化合物，能够应对白层剥落的问题，即能够应对由于润滑剂的分解而产生的氢侵入金属内部的问题。
还从金属新生面的形成对剥落产生的机制进行了说明。即，还存在下述现象：如果在金属的转动面产生磨损，则容易由于磨损而形成新生面，该形成的新生面发生催化作用，润滑脂化学分解，其结果是，产生大量的氢，产生的氢侵入钢的内部，最终在金属面中产生龟裂。专利文献2中报告了一种添加剂，通过在润滑脂中添加亚硝酸盐等钝化氧化剂来使金属表面氧化而抑制表面的催化活性，抑制因润滑剂分解所导致的氢的产生。专利文献3中报告了在钝化氧化剂中组合有机磺酸盐的技术。专利文献4中报告了在润滑脂中含有特定量的偶氮化合物的技术。专利文献5中报告了通过将润滑脂的基油设为苯基醚系合成油来抑制来自润滑脂的氢的产生的技术。
现有技术文献
专利文献
专利文献1：国际公开公报2015/016376号
专利文献2：日本特开平3-210394号公报
专利文献3：日本特开平5-263091号公报
专利文献4：日本特开2002-130301号公报
专利文献5：日本特开平3-250094号公报
发明内容
发明所要解决的课题
另一方面，已知在摩擦面中数μm至数mm的微小区域产生等离子体(Nakayama,K.,Yagasaki,F.,Tribology Letters(2018))。这样的等离子体被称为“摩擦等离子体(Triboplasma)”。有报告称，形成于滚动轴承上的润滑脂的EHL(elasto hydrodynamiclubrication，弹性流体动力润滑)薄膜中也产生放电发光、电腐蚀，由此提示EHL薄膜中产生放电等离子体(中山、田中：摩擦学会议论文集(トライボロジー会議予稿集)、东京(2016)A2)。
本发明人等认为，如果能够抑制摩擦等离子体的产生，则能够防止滚动轴承等的白层剥落。
因此本发明的课题在于，提供能够抑制滚动轴承等的白层剥落的防剥落剂和含有该防剥落剂的润滑剂组合物。
用于解决课题的方法
本发明人等使用可以作为占润滑剂组合物或润滑脂组合物较大比例的基油的化合物来测定氢产生量，结果发现，体积固有电阻率为1.0×1010Ω·cm以下的化合物能够有效抑制氢的产生。基于该见解，完成了能够有效地防止滚动轴承等的白层剥落的发明。
即，本发明提供以下的防剥落剂。
[1]一种防剥落剂，含有以防剥落剂的总质量为基准超过0.1质量％的量的、选自(A)体积固有电阻率为1.0×1010Ω·cm以下的化合物和(B)构成分子的全部碳原子中形成芳香环结构的碳原子数的比例为40％以上的化合物中的至少1种，其中，前述化合物不是丙二酸二甲酯、丁二酸二甲酯、戊二酸二甲酯、己二酸二甲酯、辛二酸二甲酯和癸二酸二甲酯中的任1种。
[2]前述第1项所述的防剥落剂，前述化合物(A)为选自在500MHz和1GHz时介电常数ε为3.0以上的化合物中的至少一种。
[3]前述第1项所述的防剥落剂，前述化合物(A)为选自汉森溶解度参数的极性力分量δp为3.5以上的化合物中的至少1种。
[4]前述第1～3中任一项所述的防剥落剂，前述化合物(A)为选自多元酯、二醇(グリコール)、硫系化合物、磷系化合物、氮系化合物、抗静电剂、离子液体、液晶中的至少1种。
[5]前述1～4中任一项所述的防剥落剂，前述化合物(A)为选自聚(氧乙烯)烷基胺、聚(氧乙烯)烷基酰胺、聚(氧乙烯)烷基醚、聚(氧乙烯)烷基苯基醚、甘油脂肪族酯、脱水山梨糖醇脂肪族酯、烷基磺酸酯、烷基苯磺酸酯、烷基磷酸酯、氯化季铵、硫酸季铵、硝酸季铵、烷基甜菜碱、烷基咪唑啉、烷基丙氨酸、聚乙烯基苄基、聚丙烯酸、胺衍生物、丁二酸衍生物、聚(氧化烯)二醇与多元醇的部分酯、烷基萘磺酸的铵化合物、聚烷基砜、烷基芳基磺酸与烷基胺的中和盐中的抗静电剂。
[6]前述1～5中任一项所述的防剥落剂，前述化合物(A)为碳原子数6以下的脂肪族一元醇与碳原子数3～10的饱和或不饱和脂肪酸、碳原子数3～10的脂环式脂肪酸或碳原子数3～10的芳香族二元酸的多元酯。
[7]前述1～6中任一项所述的防剥落剂，前述化合物(A)为选自邻苯二甲酸二甲酯、马来酸二甲酯、丙二酸二乙酯、丙二酸二丁酯和丙二酸二己酯中的多元酯。
[8]前述1～7中任一项所述的防剥落剂，前述化合物(B)为选自苯基醚、烷基苯、烷基萘中的至少1种。
本发明还提供以下的润滑剂组合物。
[9]一种润滑剂组合物，含有前述1～8中任一项所述的化合物。
[10]前述第9项所述的润滑剂组合物，进一步含有选自矿物油和合成油中的至少1种常用的基油。
[11]前述第10项所述的润滑剂组合物，前述基油为选自矿物油、合成烃油和醚油中的至少1种。
[12]前述9～11中任一项所述的润滑剂组合物，以组合物的总质量为基准，前述化合物的含量超过0.1质量％。
[13]前述9～11中任一项所述的润滑剂组合物，以组合物的总质量为基准，前述化合物的含量超过1质量％。
[14]前述9～11中任一项所述的润滑剂组合物，以组合物的总质量为基准，前述化合物的含量为2质量％以上。
[15]前述9～11中任一项所述的润滑剂组合物，以组合物的总质量为基准，前述化合物的含量为3质量％以上。
[16]前述9～11中任一项所述的润滑剂组合物，以组合物的总质量为基准，前述化合物的含量为40质量％以下。
[17]前述9～16中任一项所述的润滑剂组合物，进一步含有增稠剂。
发明效果
本发明的防剥落剂和润滑剂组合物能够有效地防止(与正十六烷相比时降低至20％以下)白层剥落。
附图说明
图1为实施例中使用的、通过摩擦等离子体来产生氢气的装置的概要图。
具体实施方式
〔定义〕
本说明书中，体积固有电阻率表示25℃时施加于试样的直流电场(V/m)与此时施加于试样的每单位截面积的电流的比，等于试样相对于边长为1cm的立方体的面间的电阻。体积固有电阻率可以基于JIS C2101中规定的电气绝缘油试验方法来测定。
本说明书中，介电常数ε是表示物质中的电荷与由此产生的力之间的关系的系数。用E4991B阻抗分析仪(Keysight Technology株式会社)在25℃下测量介电常数ε。
本说明书中，“汉森溶解度参数”是表示某溶质在某溶剂中的溶解容易度的指标，由色散项分量(δD)、极性力分量(δP)、氢键力分量(δH)3个组分构成。色散项分量(δD)表示色散力带来的效果，极性力分量(δP)表示偶极子间力带来的效果，氢键力分量(δH)表示氢键力带来的效果。汉森溶解度参数的定义和计算方法的详细信息记载于下述文献：CharlesM.Hansen著“汉森溶解度参数：用户手册(Hansen Solubility Parameters：A UsersHandbook)”，CRC出版社，2007年。
本说明书中，“白层剥落”是指伴随白色组织变化的特异性早期异常剥落。本说明书中的“白层剥落”用词与本领域中被称为白色剥落、白相剥落、脆性剥落、氢脆性剥落、氢脆化剥落等的用词意思相同。通常，对于滚动疲劳，可以以由标准(ISO281、JIS B-1518)确定的寿命计算式为基础来推测寿命。可是，在产生白层剥落这样的情况下，在与计算寿命相比短的时间内就达到寿命。在实际的市场中，有报告称，在计算寿命的约1/10～1/20时就达到寿命。白层剥落是一种内部起点型的损伤，如果用硝酸酒精液对产生后的金属组织进行蚀刻并观察，则表现出确认到白色层的特异性现象。
〔用作防剥落剂的化合物〕
本发明中使用的化合物是体积固有电阻率为1.0×1010Ω·cm以下的化合物。本发明人等发现，具有这样的物性的化合物能够抑制因等离子体所导致的氢的产生。实验方法和结果在实施例一栏有详细描述，本发明人等对于酯的碳链长对氢产生量的影响进行了系统性研究，在来自构成与甲醇的酯(R2OOC-R1-COOR2)的二元脂肪酸的碳链长(即R1)为碳原子数6以下的情况下，完全不产生氢，但碳原子数8(即二元酸为癸二酸)则会产生氢。可是，该产生量与作为标准物质使用的正十六烷相比不过为17％。认为在使用癸二酸二甲酯的情况下会产生摩擦等离子体，测定该体积固有电阻率，结果为9.0×109Ω·cm。进一步改变R1的碳原子数而测定该体积固有电阻率，结果可知，随着R1的碳原子数的増大，体积固有电阻率増大。
[表1]
Figure GDA0004016064550000051
*将正十六烷的氢产生量设为100。
另一方面，对来自构成与癸二酸的酯的醇的碳链长(即R2)对氢产生量的影响进行了研究，结果可见，随着R2的碳原子数的増大，体积固有电阻率増大。这种倾向在单酯的情况下也有观察到。
[表2]
Figure GDA0004016064550000061
*将正十六烷的氢产生量设为100。
本发明人等还发现，即使是体积固有电阻率超过1.0×1010Ω·cm的化合物，特定的芳香族化合物也能够有效地抑制氢的产生。
因此，本发明的化合物为选自(A)体积固有电阻率为1.0×1010Ω·cm以下的化合物和(B)构成分子的全部碳原子中形成芳香环结构的碳原子数的比例为50％以上的化合物中的至少1种，其中，前述化合物不是丙二酸二甲酯、丁二酸二甲酯、戊二酸二甲酯、己二酸二甲酯、辛二酸二甲酯和癸二酸二甲酯中的任1种。
(化合物(A))
作为前述化合物(A)，体积固有电阻率优选为5.0×109Ω·cm以下。
前述化合物(A)还优选25℃时为液态。
前述化合物(A)优选在500MHz(25℃)和1GHz(25℃)时介电常数ε为3.0以上。
前述化合物(A)还优选汉森溶解度参数的极性力分量δp为3.5以上。
δp用下述式表示，介电常数ε越大，δp越大。据称，一般油的介电常数ε对电子波吸收有影响，认为介电常数ε越大且介电损耗角正切越大，则越能够有效地吸收电子波，可以作为一种电子波噪声对策。
[数1]
Figure GDA0004016064550000062
已知体积固有电阻率为1.0×1010Ω·cm的化合物的δp为3.5以上。因此认为，通过δp为3.5以上，能够防止氢产生而防止白层剥落。δp优选为4.0以上。汉森溶解度参数的极性力分量δp优选为20以下。
如果δp为3.5以上，则具有能够防止静电程度的导电性，且为高介电常数，因此认为能够通过抑制摩擦等离子体的产生而抑制白层剥落，因而是优选的。
作为化合物(A)的具体例子，可列举多元酯、二醇、硫系化合物、磷系化合物、氮系化合物、抗静电剂、离子液体、液晶、SP化合物、NS化合物、脂肪酸胺盐。
多元酯选自二酯、三酯、四酯。优选为碳原子数15以下的多元酯。更优选为碳原子数15以下的二酯。其中，优选为碳原子数6以下的、更优选为碳原子数4以下的直链或支链脂肪族一元醇与碳原子数3～10的直链或支链饱和或不饱和脂肪族二元酸、碳原子数3～10的饱和或不饱和脂环式二元酸或碳原子数3～10的芳香族二元酸的二酯。特别优选为碳原子数6以下的直链或支链脂肪族一元醇与碳原子数3～10的饱和或不饱和族二元酸的二酯。最优选为碳原子数4以下的直链或支链脂肪族一元醇与碳原子数3～10的饱和或不饱和族二元酸的二酯。
作为二酯的具体例子，可列举醇为甲醇、乙醇、丙醇、丁醇或己醇、二元酸为丙二酸、丁二酸、戊二酸、己二酸、庚二酸、辛二酸、壬二酸、癸二酸、邻苯二甲酸、富马酸、马来酸、二氢粘康酸、1,4-亚苯基二乙酸或顺式4-环己烯-1,2-二羧酸的二酯。其中特别优选为醇为甲醇、乙醇、正丙醇或正丁醇、二元酸为丙二酸、丁二酸、戊二酸、己二酸、辛二酸、癸二酸、邻苯二甲酸、马来酸的二酯。特别优选为丙二酸二甲酯、丁二酸二甲酯、戊二酸二甲酯、己二酸二甲酯、辛二酸二甲酯和癸二酸二甲酯。尤其优选丙二酸二乙酯、丙二酸二丁酯和丙二酸二己酯。
作为三酯的具体例子，列举偏苯三酸三丁酯。
作为四酯的具体例子，列举季戊四醇和羧酸的全酯。优选羧酸为以2-乙基己酸、正庚酸和正辛酸为主要成分的与季戊四醇的四酯。
作为本发明中能够使用的二醇，可列举亚烷基二醇、聚亚烷基二醇或这些的烷基醚。作为亚烷基二醇，可列举四乙二醇和三丙二醇等。作为聚亚烷基二醇，可列举聚乙二醇、聚丙二醇、聚丁二醇、聚(氧乙烯)二醇、聚(氧丙烯)二醇、聚(氧丁烯)二醇、聚(氧丙烯、氧丁烯)二醇等。作为亚烷基二醇的烷基醚，可列举四乙二醇二甲基醚等。作为聚亚烷基二醇的烷基醚，可列举聚乙二醇烷基醚、聚丙二醇烷基醚(例如，聚丙二醇单丁醚)、聚丁二醇烷基醚、聚(氧化丙烯、氧化丁烯)二醇烷基醚等。烷基醚的烷基的碳原子数为1～18，可以为单醚也可以为二醚。
作为本发明中能够使用的硫系化合物是在一个分子中包含硫原子的化合物，通常用作溶剂或有机合成中的结构单元。具体地列举二甲基亚砜、2,2’-硫代二乙醇、二乙基亚砜、二丁基亚砜、丁基硫化物、丁基二硫化物、丙基硫化物、丙基二硫化物、苯基硫化物、双(2-氢甲氧基)二硫化物等。其中，优选二甲基亚砜和2,2’-硫代二乙醇。
作为本发明中能够使用的磷系化合物是在一个分子中包含磷原子的化合物，通常用作润滑油的极压剂或抗磨剂。具体地列举磷酸三甲酯、磷酸三乙酯、磷酸三丁酯、三甲基膦、三乙基膦、三丁基膦和2-乙基己基二苯基磷酸酯。其中，优选磷酸三甲酯。
作为本发明中能够使用的氮系化合物是在一个分子中包含氮原子的化合物，通常用作溶剂或有机合成中的结构单元。具体地列举甲酰胺、N-甲基甲酰胺、N-乙基甲酰胺、N-叔丁基甲酰胺，四甲基尿素、四乙基尿素、四丁基尿素等。其中，优选甲酰胺、N-甲基甲酰胺、N-叔丁基甲酰胺、四甲基尿素和四乙基尿素。
抗静电剂可以为阴离子系、阳离子系、两性系或非离子系，例如可列举化工学日报社(化学工学日報社)2018年16918的化学商品的第1238页记载的聚(氧乙烯)烷基胺、聚(氧乙烯)烷基酰胺、聚(氧乙烯)烷基醚、聚(氧乙烯)烷基苯基醚、甘油脂肪族酯、脱水山梨糖醇脂肪族酯、烷基磺酸酯、烷基苯磺酸酯、烷基磷酸酯、氯化季铵、硫酸季铵、硝酸季铵、烷基甜菜碱、烷基咪唑啉、烷基丙氨酸、聚乙烯基苄基、聚丙烯酸。另外，可列举胺衍生物、丁二酸衍生物、聚(氧化烯)二醇和多元醇的部分酯、烷基萘磺酸的铵化合物、聚烷基砜、烷基芳基磺酸与烷基胺的中和盐等。
离子液体也称为常温熔融盐，是室温下为液体的熔融盐。作为本发明中能够使用的离子液体，离子性液体的阴离子可列举选自六氟磷酸酯、三氟甲烷磺酸、双(全氟烷基磺酰基)酰亚胺、(三氟甲基磺酰基)(七氟丙基磺酰基)酰亚胺、双(氟磺酰基)酰亚胺、双五氟乙烷磺酸酰亚胺、三氧化氮、对甲苯磺酸、二乙二醇单甲基醚磺酸、乙酸、三氟甲烷羧酸、双氰基酰亚胺和三三氟甲烷磺酸甲酯、三(全氟烷基)三氟磷酸酯、双(全氟烷基)(三氟甲基)三氟磷酸酯中的物质。
例如，阴离子可以更优选使用下述式1或2中任一个所表示的离子液体。
(Rf1-SO2)(Rf2-SO2)N- 式1
(Rf3)(Rf3)(Rf3)PF3 - 式2
式1中，Rf1和Rf2相互可以相同也可以不同，表示F、CF3、C2F5、C3F7或C4F9。式2中，Rf3相互可以相同也可以不同，表示CF3、C2F5、C3F7或C4F9。
作为式1所表示的阴离子，可列举双(全氟烷基磺酰基)酰亚胺、(三氟甲基磺酰基)(七氟丙基磺酰基)酰亚胺、双(氟磺酰基)酰亚胺等。作为式2所表示的阴离子，可列举三(全氟烷基)三氟磷酸酯、双(全氟烷基)(三氟甲基)三氟磷酸酯等。
作为构成离子液体的阳离子，为咪唑
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作为本发明中能够使用的离子液体，优选为阴离子为双(三氟甲基磺酰基)酰亚胺、阳离子为1-丁基-2,3-二甲基咪唑
Figure GDA00040160645500000924
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液晶化合物是在某一温度区域中外观上为液体、同时显示光学各向异性晶体所特有的双折射性的化合物。液晶化合物根据其熔融状态分为近晶液晶、向列液晶、胆甾液晶、碟型液晶，本发明中，它们中的任一液晶化合物均可使用。
作为本发明中使用的液晶化合物的具体例子，可列举以下所示那样的(1)席夫碱系、(2)偶氮系、氧化偶氮系、(3)苯甲酸酯系、(4)联苯基系、三联苯系、(5)环己基羧酸酯系、(6)苯基环己烷系、联苯基环己烷系、(7)嘧啶系、二
Figure GDA0004016064550000101
烷系、(8)环己基环己烷酯系、(9)环己基乙烷系、(10)环己烷系、(11)TRAN系、(12)胆甾系、(13)三嗪系、(14)COS系、(15)CCN系、(16)碟型液晶等。
前述(4)的氰基联苯基系液晶化合物化学稳定性优异，但液晶相的温度范围有点窄，优选与其他液晶化合物混合使用，是介电常数各向异性高的向列液晶，大量用于液晶显示器。例如，作为氰基联苯基系液晶，可列举4-氰基-4'-戊基联苯、4-氰基-4'-丁基联苯、4-氰基-4'-己基联苯、4-氰基-4'-庚基联苯、4-氰基-4'-辛基联苯、4-氰基-4'-壬基联苯、4-氰基-4'-十一烷基联苯、4-氰基-4'-十二烷基联苯、4-丁氧基-4'-氰基联苯、4-乙氧基-4'-氰基联苯、4-丙氧基-4'-氰基联苯、4-戊氧基-4'-氰基联苯、4-己氧基-4'-氰基联苯、4-庚氧基-4'-氰基联苯、4-辛氧基-4'-氰基联苯、4-壬氧基-4'-氰基联苯、4-癸氧基-4'-氰基联苯、4-十二烷氧基-4'-氰基联苯、(S)-4-氰基-4'-(2-甲基丁基)联苯、4-(反式4-丙基环己基)苯甲腈、4-(反式4-丁基环己基)苯甲腈、1-(反式4-戊基环己基)-4氰基苯、4-[反式4-[(E)-1-丙烯基]环己基]苯甲腈、4-氰基-4”-戊基-对三联苯、4-氰基-4”-丙基-对三联苯、反式4'-(4-戊基环己基)联苯基-4-腈。
作为本发明中能够使用的SP化合物是在一个分子中包含硫原子和磷原子的化合物，通常用作润滑油的极压剂或抗磨剂。具体地列举烷基化硫代磷酸三苯酯和ZnDTP。其中，优选烷基化三苯基硫代磷酸酯。
作为本发明中能够使用的NS化合物是在一个分子中包含氮原子和硫原子的化合物，通常用作润滑油的金属腐蚀抑制剂。具体地列举二巯基噻二唑衍生物、二硫代氨基甲酸钼、ZnDTC等。其中，优选二巯基噻二唑衍生物和二硫代氨基甲酸钼。
作为本发明中能够使用的脂肪酸胺盐是通常用作润滑油的防锈剂的化合物。具体地，可以列举油酸二环胺盐、月桂酸胺盐、肉豆蔻酸胺盐、棕榈酸胺盐、硬脂酸胺盐、亚油酸胺盐、花生四烯酸胺盐、亚麻酸胺盐等。其中，优选油酸二环胺盐。
(化合物(B))
化合物(B)是构成分子的全部碳原子中形成芳香环结构的碳原子数的比例为40％以上、优选50％以上、更优选60％以上的化合物。
在此，可以通过计算来求出构成分子的全部碳原子中形成芳香环结构的碳原子数的比例。例如，在二苯胺的情况下，全部碳原子数为13，形成芳香环结构的碳原子数为12。因此，将12除以13所获得的值即为前述比率。
作为化合物(B)，优选具有两个以上芳香环的烷基化合物或烯基化合物。作为具体例，列举二苯甲烷、二苯丙烷和二苯基乙烯。还优选具有3个以上芳香环的苯基醚，优选五苯基醚、四苯基醚、烷基四苯基醚等苯基醚、烷基苯、烷基萘。
本发明的防剥落剂只要不会不利地影响前述化合物(A)或(B)的防剥落离效果即可含有任何物质，但以本发明的防剥落剂的总质量为基准，前述化合物的含量优选为1质量％以上，更优选为2质量％以上，进一步优选为3质量％以上。作为前述化合物，在使用化合物(A)和化合物(B)中任一方的情况下，与前述化合物同样，其含量超过0.1质量％，优选超过1质量％，更优选为2质量％以上，进一步优选为4质量％以上。在将化合物(A)与化合物(B)并用的情况下，其合计量优选为2％以上，更优选为4％以上。本发明的防剥落剂中前述化合物的比例的上限没有特别限制。在多元酯和二醇的情况下，从耐热性、耐树脂性的观点出发，相对于防剥落剂的总质量，优选小于40质量％，更优选小于10质量％。从经济性观点出发，在多元酯和二醇以外的化合物的情况下，优选为10质量％以下，更优选为3质量％以下。
存在由于伴随润滑部的摩擦产生的等离子体而起火的危险性，因此本发明化合物的闪点(引火点)优选为70℃以下。闪点可以基于JIS K2265来测定。
〔润滑剂组合物〕
前述化合物常温下为液体，因此可以单独制成润滑剂组合物，也可以作为润滑剂或润滑脂的基油来使用，还可以与作为润滑剂或润滑脂的基油的常用的基油混合来制成润滑剂组合物。
(常用的基油)
作为前述常用的基油，可以使用体积固有电阻率超过1.0×1010Ω·cm的基油。优选为含有总碳原子数为12以上的饱和或不饱和烃基的基油，具体地，可列举矿物油或合成油。作为矿物油，可以使用石蜡系矿物油、环烷系矿物油、它们的混合物。优选含有高精制矿物油(即通过脱蜡处理来减少低温时蜡成分的析出，由此使流动点比未精制的矿物油的流动点(-5℃～-20℃水平，基于JIS K 2269测定)低的矿物油)。作为合成油，可列举合成烃油、酯油、醚油、二醇、硅油、氟化油等。作为合成烃油，可列举聚α烯烃(PAO)、聚丁烯等。其中优选为聚α烯烃。作为酯油，可列举二酯、偏苯三酸酯、多元醇酯等。作为醚油，可列举烷基二苯基醚(ADE)、二烷基二苯基醚、聚丙二醇等。作为二醇，可列举聚丙二醇、聚丙烯烷基醚等。
如果与矿物油或合成烃油(尤其是聚α烯烃)并用，则即使前述化合物为少量，例如以润滑剂组合物的总质量为基准超过0.1质量％、优选为超过1质量％、更优选为2质量％以上、进一步优选为3质量％以上，也能够有效抑制氢的产生。本发明的润滑剂组合物中前述化合物的含量例如为40质量％以下，可以是20质量％以下、10质量％以下、5质量％以下或3质量％以下。考虑到与前述化合物的相容性，作为常用的油，优选为二酯、多元醇酯等酯油、烷基苯基醚油等醚油、非水溶性的聚亚烷基二醇等二醇、硅油、氟化油等。从耐树脂性、耐热性的观点出发，优选为矿物油、合成烃油或苯基醚油、烷基苯基醚油。
本发明的润滑剂组合物中基油(即前述化合物(A)和/或(B)单独或与前述常用的油的混合油)的40℃时的运动粘度优选为10～500mm2/s。如果基油40℃时的运动粘度低于10mm2/s，则存在低速、高温时无法确保充分的油膜的情况，此外，如果超过500mm2/s，则存在高速、低温时发生扭矩上升的可能。出于同样的理由，更优选为50～200mm2/s，进一步优选为60～130mm2/s。其中，基油的运动粘度可以基于JIS K2283来测定。
本发明的润滑油组合物中的基油的含量，相对于基油和防剥落剂的合计100质量份，优选为60～99.9质量份，更优选为90～99.9质量份，进一步优选为97～99.9质量份。如果基油的含量在该范围内，则润滑性优异且挥发性低，因而优选。
(任选的添加剂)
根据需要，本发明的润滑剂组合物可以进一步含有通用的添加剂。例如，根据需要，可以含有防锈剂、耐负荷添加剂、抗氧化剂等。以本发明润滑剂组合物的总质量为基准，这些任选的添加剂的含量通常为0.5～5质量％。
作为防锈剂，可列举无机系防锈剂和有机系防锈剂。作为无机系防锈剂，可列举硅酸Na、碳酸Li、碳酸K、氧化Zn等无机金属盐。作为有机系防锈剂，可列举苯甲酸Na、苯甲酸Li等苯甲酸盐、磺酸钙、磺酸锌等磺酸盐、环烷酸Zn、癸二酸Na等羧酸盐、丁二酸、丁二酸酐、丁二酸半酯等丁二酸衍生物、山梨糖醇单油酸酯、脱水山梨糖醇三油酸酯等脱水山梨糖醇酯、脂肪酸胺盐。
作为耐负荷添加剂，可列举磷酸酯等磷系、多硫化物、硫化润滑脂等硫系、硫代磷酸酯等磷-硫系、硫代氨基甲酸盐、硫代磷酸盐、有机磷酸酯。
抗氧化剂可列举作为润滑脂的氧化劣化抑制剂广为人知的酚系抗氧化剂、胺系抗氧化剂。
作为酚系抗氧化剂，可列举2,6-二-叔丁基-p-甲酚(BHT)、2,2’-亚甲基双(4-甲基-6-叔丁基酚)、4,4’-亚丁基双(3-甲基-6-叔丁基酚)、2,6-二-叔丁基-酚、2,4-二甲基6-叔丁基酚、叔丁基羟基苯甲醚(BHA)、4,4’-亚丁基双(3-甲基-6-叔丁基酚)、4,4’-亚甲基双(2,3-二-叔丁基酚)、4,4’-硫代双(3-甲基-6-叔丁基酚)、十八烷基-3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯等。其中优选为十八烷基-3-(3,5-二-叔丁基-4-羟基苯基)丙酸酯。
作为胺系抗氧化剂，可列举N-正丁基-对氨基酚、4,4’-四甲基-二-氨基二苯基甲烷、α-萘基胺、N-苯基-α-萘基胺、吩噻嗪、烷基二苯基胺等。其中优选为烷基二苯基胺。
本发明的润滑剂组合物能够作为润滑油、导电性油、动压油等使用。本发明的润滑剂组合物对防止剥落磨损是有效的。
〔润滑脂组合物〕
本发明的润滑剂组合物也可以进一步含有增稠剂来制成润滑脂组合物。
出于与润滑剂组合物所述相同的原因，基于本发明的润滑脂组合物的总质量，前述化合物(A)和/或(B)的含量优选超过0.1质量％，更优选超过1质量％，进一步优选2质量％以上，特别优选3质量％以上，并且，上限例如可以是40质量％以下、20质量％以下、10质量％以下、5％质量以下或3质量％以下。
作为本发明的润滑脂组合物中能够使用的增稠剂，可列举二脲所代表的脲系增稠剂、Li皂、Li复合皂所代表的Li皂系增稠剂、膨润土、硅胶等固体增稠剂等。优选为脲系增稠剂和Li皂系增稠剂。
根据需要，本发明的润滑脂组合物可以进一步含有通用的添加剂。作为能够使用的添加剂，可列举关于润滑剂组合物记载的物质。基于本发明的润滑脂组合物的总质量，任选的添加剂的含量通常为0.1～5质量％。
(锥入度)
本发明的润滑脂组合物的混合锥入度优选为200～300，更优选为220～280。如果混合锥入度超过300，则高速旋转导致的泄漏增加，有时无法满足足够的润滑寿命。另一方面，如果混合锥入度低于200，则润滑脂的流动性变差，有时无法满足足够的润滑寿命。需说明的是，在本说明书中，术语“锥入度”是指60次混合锥入度。锥入度可以根据JIS K2220 7来测定。
(增稠剂的含量)
以本发明润滑脂组合物的总质量为基准，增稠剂的含量优选为5～25质量％，更优选为10～20质量％。如果低于5质量％，则有时润滑脂变软、泄漏，存在无法满足足够的润滑寿命的情况。另一方面，如果比25质量％多，则流动性变差，因此，润滑脂难以进入润滑部，存在无法满足足够的润滑寿命的情况。
(基油的含量)
基于本发明的润滑脂组合物的总质量，基油的含量优选为60～90质量％，更优选为70～90质量％。如果基油的含量在该范围内，则润滑性优异且挥发性低，因而优选。
〔轴承〕
本发明的润滑脂组合物用于产业机械用、汽车用的各种滚动轴承。作为产业机械用，可列举例如产业机械用各种马达、产业用机器人的减速机、油压设备、风力发电装置的主轴、减速机、电梯的起重机周边的滚动轴承。作为汽车用，优选为汽车电气设备、辅机用滚动轴承。作为汽车电气设备、辅机，可列举交流发电机、车载空调用电磁离合器、中间皮带轮、惰轮、张紧轮等。
实施例
〔氢产生试验和氢产生量的测定〕
利用纳山、中山等“摩擦学会议论文集，东京(2017)185”中记载的方法，测定氢产生量。
具体地，使用能够在针/平板电极间产生摩擦等离子体的摩擦等离子体产生装置(图1)。针为阴极，平板为阳极。针的材质为SCM435钢，针的顶角为120°。针相对于阳极平板垂直配置，固定在针的前端与阳极上表面的距离为50μm的位置。针与平板电极的距离利用千分尺来控制。阳极平板的材质为SPCC钢。阳极平板构成容器内部的底部。在该容器中投入实施例或比较例的防剥落剂等，针与容器内部的防剥落剂等接触。阳极平板与阴极针通过高压电源连接。施加电压时的电压和电流可以用示波器测量。容器与针以覆盖两者的方式被更大的壳体(以下称为“气氛控制槽”)包围。该气氛控制槽的顶部设有开口部，可以经由微型注射器采集气氛控制槽内部的气体。该气氛控制槽的侧部上方也设有开口部，可以导入干燥空气。气氛控制槽内部的气体可以用半导体式传感器来检测。
导入30秒干燥空气，与气氛控制槽内部的气体进行置换。在气氛控制槽内部的气体置换为干燥空气后，利用示波器监测电流值和电压值并进行30秒放电，然后静置20秒，用微型注射器采集所产生的气体。将采集的气体导入气相色谱，测定氢气量。需说明的是，气相色谱使用气相色谱仪GC-2010(岛津制作所制)、色谱柱使用
Figure GDA0004016064550000161
检测器使用TCD进行测定。将正十六烷的氢产生量设为100％，算出各化合物的氢产生量。
将结果示于表3～10。实施例1～38是防剥落剂的实施例，实施例39～71是含有防剥落剂的润滑油组合物的实施例。实施例42是3.0质量％实施例3的丙二酸二甲酯和97.0质量％比较例8的聚α烯烃的混合物，表明即使混合物的体积固有电阻率超过1.0×1010Ω·cm，只要含有规定量的体积固有电阻率为1.0×1010Ω·cm以下的本申请的防剥落剂，也能够将氢产生量控制在0％。
表3
Figure GDA0004016064550000171
表4
Figure GDA0004016064550000181
表5
Figure GDA0004016064550000191
表6
Figure GDA0004016064550000201
表7
Figure GDA0004016064550000211
表8
Figure GDA0004016064550000221
表9
Figure GDA0004016064550000231
表10
Figure GDA0004016064550000241
将实施例和比较例中使用的化合物的供应者和商品名示于下文。
Figure GDA0004016064550000251
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Claims (7)

1.一种含有防剥落剂的润滑剂组合物，所述防剥落剂含有选自(A)体积固有电阻率为1.0×1010Ω·cm以下的化合物和(B)构成分子的全部碳原子中形成芳香环结构的碳原子数的比例为40％以上的化合物中的至少1种，
其中，所述化合物不是丙二酸二甲酯、丁二酸二甲酯、戊二酸二甲酯、己二酸二甲酯、辛二酸二甲酯和癸二酸二甲酯中的任1种，
以组合物的总质量为基准，所述化合物的含量超过0.1质量％且40质量％以下，
所述化合物(A)为选自由多元酯、二醇、氮系化合物、离子液体、液晶组成的组中的至少1种，
所述多元酯为选自由邻苯二甲酸二甲酯、马来酸二甲酯、丙二酸二乙酯、丙二酸二丁酯和丙二酸二己酯组成的组的至少1种，
所述二醇为亚烷基二醇、聚亚烷基二醇或这些的烷基醚，所述亚烷基二醇为选自由四乙二醇和三丙二醇组成的组的至少1种，所述聚亚烷基二醇为选自由聚丁二醇、聚(氧乙烯)二醇、聚(氧丙烯)二醇、聚(氧丁烯)二醇和聚(氧丙烯、氧丁烯)二醇组成的组的至少1种，所述亚烷基二醇的烷基醚为四乙二醇二甲基醚，所述聚亚烷基二醇的烷基醚为选自由聚乙二醇烷基醚、聚丙二醇烷基醚、聚丁二醇烷基醚和聚(氧化丙烯、氧化丁烯)二醇烷基醚组成的组的至少1种，
所述氮系化合物为选自由甲酰胺、N-甲基甲酰胺、N-乙基甲酰胺、N-叔丁基甲酰胺、四甲基尿素、四乙基尿素和四丁基尿素组成的组的至少1种，
所述离子液体为选自由阴离子为双(三氟甲基磺酰基)酰亚胺、阳离子为1-丁基-2,3-二甲基咪唑
Figure FDA0004016064540000011
的离子液体，阴离子为双(三氟甲基磺酰基)酰亚胺、阳离子为1-(2-甲氧基乙基)-1-甲基吡咯烷
Figure FDA0004016064540000012
的离子液体，阴离子为双(三氟甲基磺酰基)酰亚胺、阳离子为三乙基辛基
Figure FDA0004016064540000013
的离子液体，阴离子为(三氟甲基磺酰基)(七氟丙基磺酰基)酰亚胺、阳离子为1-乙基-3-甲基咪唑
Figure FDA0004016064540000014
的离子液体以及N-(甲氧乙基)-1-甲基吡咯烷
Figure FDA0004016064540000015
双(三氟甲基磺酰基)酰亚胺组成的组中的至少1种，
所述液晶是氰基联苯基系液晶，
所述化合物(B)为选自由二苯甲烷、二苯丙烷和二苯基乙烯组成的组中的至少一种。
2.根据权利要求1所述的润滑剂组合物，进一步含有选自矿物油和合成油中的至少1种基油。
3.根据权利要求2所述的润滑剂组合物，所述基油为选自矿物油、合成烃油和醚油中的至少1种。
4.根据权利要求1～3中任一项所述的润滑剂组合物，以组合物的总质量为基准，所述化合物的含量超过1质量％。
5.根据权利要求1～3中任一项所述的润滑剂组合物，以组合物的总质量为基准，所述化合物的含量为2质量％以上。
6.根据权利要求1～3中任一项所述的润滑剂组合物，以组合物的总质量为基准，所述化合物的含量为3质量％以上。
7.根据权利要求1～3中任一项所述的润滑剂组合物，进一步含有增稠剂。
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