CN1117839C - 润滑油组合物 - Google Patents

润滑油组合物 Download PDF

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Publication number
CN1117839C
CN1117839C CN98808718A CN98808718A CN1117839C CN 1117839 C CN1117839 C CN 1117839C CN 98808718 A CN98808718 A CN 98808718A CN 98808718 A CN98808718 A CN 98808718A CN 1117839 C CN1117839 C CN 1117839C
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base
lubricating oil
composition
engine
oil
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CN1268969A (zh
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R·罗伯森
T·A·布莱泰尔
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Infineum USA LP
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Infineum USA LP
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Abstract

一种用于内燃机的润滑油组合物含有：(A)主要量的润滑粘度基料，该基料含有大于35-小于70质量%的一种或多种PAO，其余的基料优选是一种或多种如在APO中定义的I类基料；和(B)两种或多种添加剂组分例如无灰分散剂和金属清净剂。

Description

润滑油组合物
本发明涉及用于内燃机曲轴箱的润滑油组合物。
内燃机制造商对机动车辆发动机中使用的曲轴箱润滑油的要求更换周期的增长感兴趣，该周期用英里数或时间表示。润滑油配方设计师针对这个问题并设计了一些试验，这些试验是测量润滑油在曲轴箱中比目前保持使用更长的英里数或时间。这种试验被称作“长换油适应性试验”。这种试验的一个例子是对汽油机的VW PV 1449试验。
本发明涉及通过提供一种在润滑油组合物中确定的基料，在不需使用昂贵的、专门的配方的条件下改善在“长换油适应性试验″中的性能。
用于润滑油组合物中有时称作基础油的基料可以包括合成的或天然的油，该油用作点燃式和压燃式发动机的曲轴箱润滑油。该润滑油基料的运动粘度在100℃下一般为2.5-12mm2/秒，优选2.5-9mm2/秒。基料的粘度特性一般用油的中性值(neutral number)(例如S150N)表示，在给定的温度下中性值越高，粘度越高。该值定义为在SayboltUniversal Seconds中测定的40℃下的基料的粘度。直馏馏分混合物的平均基料的中性值(平均BSNN)可根据下列公式确定：
Figure C9880871800031
其中BSRn＝基料n的基料比
        ＝(基料n重量％/油中总基料重量％)×100％
   BSNNn＝基料n的基料中性值
具有较低的溶剂中性值的基料被用于较低的粘度等级。例如，一般的基料将具有90-180的BSNN。
GB-A-2292747描述了含有极性分散剂和含有20-70％、特别是35-20％、优选15-25％的PAO(聚α烯烃)油的基油的汽车曲轴箱润滑油。其指出该润滑油优选含有清净剂。还指出该润滑油可与用于发动机密封的碳氟化合物和腈材料相配伍。
然而，GB-A-2292747所述的润滑油的问题是，当润滑油含有在此所指定的百分数量的PAO时，正如在此所证明的那样，在较低的所述PAO百分数下，它们将会在发动机试验中引起粘度的增高，或者在高的所述PAO百分数下其变得昂贵。
本发明涉及使用中等量的PAO以解决上述问题。
因此，本发明的第一方面是用于内燃机的润滑油组合物，该组合物含有：
(A)一种主要量的润滑粘度的基料，该基料含有大于35-小于70，例如37-68，优选40-60％(质量)的一种或多种IV类基料。和
(B)两种或多种添加剂组分。
优选的是，其余的基料是一种或多种选自I类基料的基料。I和IV类基料定义如下。
优选该基料含有大于40-小于60，例如42-58，优选45-55％(质量)所述一种或多种IV类基料。
本发明的第二方面是制备润滑油组合物的方法，该方法包括混合(A)和(B)，每个(A)和(B)的定义与第一方面的相同。
本发明的第三方面是运行内燃机，例如点燃式发动机的方法，该方法包括用第一方面的润滑油组合物或由第二方面的方法制备的润滑油组合物润滑发动机。
本发明的第四方面是使更换点燃式发动机中曲轴箱润滑油的周期增长，该方法包括用润滑油组合物处理运动的表面，该润滑油组合物含有下述(A)和(B)，或者通过混合(A)和(B)制备。
(A)主要量的润滑粘度基料，该基料含有25-80，例如25-70％(质量)一种或多种如本文所定义的IV类基料，或它们的混合物；和
(B)两种或多种添加剂组分，例如第一方面的添加剂组分，或者由第二方面的方法制备的添加剂组分。
下面更详细地论述本发明的特征。
(A)基料
基料的粘度在100℃下适合在2-20，例如2.5-12cSt，较好2.5-9cSt(100℃下)，优选3-7cSt(100℃下)。
可用各种不同的方法制备基料，这些方法包括(但不限于)蒸馏，溶剂精制，加氢处理，低聚反应，酯化，和再精制。API 1509“发动机润滑油使用许可和检验体系″第十四版，1996年12月，指出所有的基料被分成5种常规种类：
I类含有小于90％饱和化合物和/或大于0.03％硫，并具有粘度指数大于或等于80和小于120；
II类含有大于或等于90％饱和化合物和小于或等于0.03％硫，并且具有粘度指数大于或等于80和小于120；
III类含有大于或等于90％饱和化合物和小于或等于0.03％硫，并且具有粘度指数大于或等于120；
IV类是聚α烯烃(PAO)；和
V类包括不包括在I，II，III或IV类中的所有的基料。
用于定义上述种类的试验方法是检测饱和化合物的ASTM D2007；检测粘度指数的ASTM D2270；和检测硫的ASTM D2622，4294，4927和3120。
IV类基料，即聚α烯烃(PAO)包括α-烯烃的氢化低聚物，低聚反应的最重要的方法是自由基方法，Ziegler催化，和阳离子，Friedel-Crafts催化。
聚α烯烃的粘度一般为2-20cSt(100℃)，优选为4-8cSt(100℃)。它们可以是，例如具有2-16个碳原子的支链或直链α-烯烃的低聚物，具体的例子是聚丙烯，聚异丁烯，聚-1-丁烯，聚-1-己烯，聚-1-辛烯和聚-1-癸烯。包括均聚物，共聚体和混合物。PAO描述在“润滑油的化学和工艺(Chemistry and Technology of Lubricants)”中，R.M.Mortier和S.T.Orszulik编辑，Blackie(Glasgow)and VCH Publishers Inc.N.Y.(1992)出版：Ch2合成基液。
关于其他的上述基料，“I类基料”还包括与一种或多种其他类基料混合的I类基料，但须得到的混合物具有I类基料的上述特征。
(B)添加剂组分
添加剂组分的例子如下：
无灰分散剂
无灰分散剂的例子是高分子量无灰分散剂，包括为了减少汽油机或柴油机中沉积物形成可有效加入到润滑油中的已知无灰分散剂。“高分子量”是指数均分子量为700-5000，例如1300-1400。如下面所详细描述的那样，可得到各种这样的化合物。
该无灰分散剂包括油溶性的聚合烃，其主链具有能够与要分散的粒子结合的官能团。通常，分散剂包括极性部分通常通过桥基连接到聚合物主链上的胺，醇，酰胺或酯。例如，该无灰分散剂可选自长链烃取代的单和二羧酸或其酐的油溶性盐，酯，氨基酯，酰胺，酰亚胺和噁唑啉；长链烃的硫代羧酸盐衍生物；具有与其直接连接的聚胺的长链脂族烃；和通过长链取代的酚与甲醛和聚亚烷基聚胺缩合形成的Mannich缩合产物。
聚合烃与不饱和羧酸、酐或酯反应的方法和从这些化合物制备衍生物的方法公开在US-A-3087936，US-A-3172892，US-A-3215707，US-A-3231587，US-A-3231587，US-A-3272746，US-A-3275554，US-A-3381022，US-A-3442808，US-A-356804，US-A-3912764，US-A-4110349，US-A-4234435和GB-A-1440219。
一类无灰分散剂包括使用新的金属茂催化剂化学作用制备的亚乙基α-烯烃共聚物和α-烯烃均聚物和共聚物，这些聚合物可以具有高度的(例如＞30％)末端亚乙烯基不饱和，这些聚合物描述在US-A-5128056，5151204，5200103，5225092，5266223，5334775；WO-A-94/19436，94/3709；和EP-A-440506，513157，513211。正如CCS粘度与kV100℃之比所表示的，所述的这些分散剂具有优良的测粘性质。
本文所用的术语“α-烯烃”表示下式的烯烃
Figure C9880871800071
其中R′优选是C1-C18烷基。对末端亚乙烯基不饱和的要求是指存在下列结构式的聚合物：
Figure C9880871800072
其中Poly是聚合物链，R一般是C1-C18烷基，通常是甲基或乙基。优选该聚合物将具有至少50％，最优选至少60％具有末端亚乙烯基不饱和的聚合物链。如WO-A-94/19426所示，乙烯/1-丁烯共聚物一般具有不多于链的约10％的末端乙烯基和该链其余部分的内部单不饱和基团。不饱和性质可通过FTIR光谱分析，滴定或C-13 NMR确定。
油溶性聚合烃主链可以是两种或多种这样的烯烃的均聚物(例如，聚丙烯)或共聚物(例如，乙烯和α烯烃例如丙烯或丁烯的共聚物，或两种不同的α烯烃的共聚物)。其他共聚物包括其中较少量的，例如1-10摩尔％的共聚物单体是α，ω二烯烃，例如C3-C22非共轭的二烯烃的那些共聚物(例如异丁烯和丁二烯的共聚物，或乙烯，丙烯和1，4-己二烯或5-亚乙基-2-降冰片烯的共聚物)。也可使用通常具有 Mn为700-5000的无规立构丙烯低聚物，例如描述在EP-A-490454中的低聚物以及杂聚合物例如聚环氧化物。
一类优选的烯烃聚合物是聚丁烯，特别是聚正丁烯，例如可通过C4炼油厂物流聚合制备的聚合物。优选的其他类烯烃聚合物是EAO共聚物，该共聚物优选含有1-50摩尔％乙烯，更优选5-48摩尔％乙烯。这样的聚合物可以含有多于一种α烯烃并且可以含有一种或多种C3-C22二烯烃。也可使用各种乙烯含量的EAO混合物。也可混合或掺合不同类型的聚合物，例如EAO，以及 Mn不同的聚合物；也可以混合或掺合由这些聚合物衍生的组分。
用于本发明所用的分散剂中的烯烃聚合物和共聚物优选具有 Mn为700-5000，更优选1300-4000。聚合物分子量，特定的Mn，可用不同的已知方法确定。一种常规方法是凝胶渗透色谱法(GPC)，该方法还提供了分子量分布情况(见W.WW.Yau J.J.kirkland和D D.Bly，“Modern Size Exclusion Liquid Chromatography”，John Wiley和Sons，纽约，1979)。另一种特别对较低分子量聚合物有效的方法是蒸气压渗透压力测定法(见例如ASTM D3592)。
聚合物的聚合度Dp是： D p = Σ i Mn × mol . % monomeri 100 × mol . wtmonomeri
因此对两个单体的共聚物的Dp可用下式计算： D p = Mn × mol . % monomer 1 100 × mol . wtmonomer 1 + Mn × mol . % monomer 2 - 100 × mol . wtmonomer 2
优选的是，用于本发明的聚合物主链的聚合度为至少45，一般为50-165，更优选55-140。
特别优选的共聚物是乙烯丁烯共聚物。优选的是，烯烃聚合物和共聚物可以通过不同的催化聚合方法制备，该催化聚合方法使用金属茂催化剂，该催化剂是例如下式的体积庞大的(bulky)配位体过渡金属化合物：
         [L]mM[A]n
其中L是体积配位体；A是离去基团，M是过渡金属，m和n是这样的以致总的配位体价等于过渡金属价。优选催化剂是4个配位的以致该化合物可电离成1+价态。
配位体L和A可以彼此桥连，如果存在两个配位体A和/或L，则它们可以桥连。金属茂化合物可以是具有两种或多种配位体L的全夹层化合物，配位体L可以是环戊二烯基配位体或环戊二烯基衍生的配位体，或者它们可以是具有一种这种配位体L的半夹层化合物。该配位体可以是单-或多环的或任何其他可η-5键合到过渡金属的配位体。
一种或多种配位体可以π-键合到过渡金属原子上，该过渡金属可以是4，5或6族过渡金属和/或稀土元素或锕系元素过渡金属，特别优选锆，钛和铪。
配位体可以被取代或未取代的，并且可以是单-，二-，三-，四-和五取代的环戊二烯基环。任意的取代基可在配位体和/或离去基团和/或过渡金属之间作为1个或多个桥。这样的桥一般包括一个或多个含有碳，锗，硅，磷或氮原子的基团，优选该桥接入1个原子以连结被桥连的实体之间，虽然该原子可以且常常带有其他取代基。
金属茂还可以含有其他可替换的配位体，优选用助催化剂(离去基团)替换，该助催化剂通常选自多种多样的烃基和卤素。
这样的聚合，催化剂，和助催化剂或活化剂描述在，例如US-A-4530914，4665208，4808561，4871705，4897455，4937299，4952716，5017714，5055438，5057475，5064802，5096867，5120867，5124418，5153157，5198401，5227440，5241025；EP-A-129368，277003，277004，420436，520732；和WO-A-91/04257，92/00333，93/08199，93/08221，94/07928和94/13715。
可官能化油溶性聚合烃主链以引入官能团到该聚合物的主链，或者该官能团作为一个或多个聚合物主链上的侧基。该官能团一般是极性的，并含有一个或多个杂原子例如P，O，S，N，卤素或硼。可通过取代反应将官能团连接到油溶性的聚合烃主链的饱和烃部分，或通过加成或环加成连接到烯烃部分。做为选择也可以通过聚合物链端的氧化或解离(例如，如臭氧分解那样)将该官能团引入到聚合物中。
有效的功能化反应包括：在烯键卤化聚合物，随后该卤化聚合物与乙烯不饱和官能化合物反应(例如，马来酸化，其中聚合物与马来酸或酐反应)；通过不经卤化的“烯(ene)”反应聚合物与不饱和官能化合物反应；聚合物与至少一种酚基(它可以在曼尼希碱型缩合中衍生)反应；使用Koch型反应在不饱和这一点上聚合物与一氧化碳反应以便在异或新位置上引入羰基；使用自由基催化剂通过自由基加成使聚合物与官能化化合物反应；与硫代羧酸衍生物反应；通过空气氧化方法，环氧化作用，氯代氨基化或臭氧分解反应该聚合物。
然后该官能化油溶性聚合烃主链与亲核反应物例如胺，氨基醇，醇，金属化合物或其混合物进一步衍生形成相应的衍生物。对衍生官能化聚合物有效的胺化合物包括至少一种胺，并且可以包括一种或多种另外的胺或其他的反应性或极性基团。这些胺可以是烃基胺或主要是烃基胺，其中烃基包括其他的基团，例如羟基，烷氧基，酰胺基，腈，咪唑啉基等等。特别有效的胺化合物包括单-和聚胺，例如在分子中有约2-60，合宜地2-40(例如3-20)总碳原子和约1-12，合宜地3-12，优选3-9个氮原子的聚亚烷基聚胺和聚亚氧烷基聚胺。可以有利地使用胺化合物的混合物例如亚烷基二卤化物与氨反应制备的那些混合物。优选的胺是脂肪族饱和的胺，包括例如1，2-二氨基乙烷；1，3-二氨基丙烷；1，4-二氨基丁烷；1，6-二氨基己烷；聚乙烯胺例如二亚乙基三胺；三亚乙基四胺；四亚乙基五胺；和聚亚丙基胺例如1，2-亚丙基二胺化合物；和二-(1，2-亚丙基)三胺。
其他有效的胺化合物包括：脂环族二胺例如1，4-二(氨基甲基)环己烷，杂环氮化合物例如咪唑啉。特别有效的一类胺是聚酰氨基和有关的酰氨基-胺，例如公开在US4,857,217；4,956,107；4,963,275；和5,229,022。还可使用的胺是如US4,102,798；4,113,639；4,116,876；和UK989,409中所述的三(羟甲基)氨基甲烷(THAM)。也可使用Dendrimers，星状胺和梳状结构状胺。同样地，可以使用公开在US5,053,152中的缩合胺。根据EP-A208560；US4,234,435和US5,229,022所述的常规方法，官能化聚合物与胺化合物反应。
该官能化油溶性聚合烃主链也可以用羟基化合物例如一元醇和多元醇或用芳香族化合物例如酚和萘酚衍生。优选多元醇，例如，其中亚烷基含有2-8个碳原子的亚烷基二醇。其他有效的多元醇包括甘油，甘油的单油酸酯，甘油的一硬脂酸酯，甘油的单甲基醚，季戊四醇，二季戊四醇及其混合物。酯分散剂也可以由不饱和的醇例如烯丙基醇，肉桂基醇，炔丙基醇，1-环己烷-3-醇和油醇制得。能够形成无灰分散剂的其他种类的醇包括醚-醇，并包括例如氧化亚烷基，氧化亚芳基。它们的例子是具有高达150个氧化亚烷基的醚-醇，其中亚烷基含有1-8个碳原子。该酯分散剂可以是琥珀酸的二酯或酸性酯，即部分酯化的琥珀酸，以及部分酯化的多元醇或酚，即具有游离醇或酚式羟基的酯。酯分散剂可以通过例如US3381022中所述的一些已知方法中的一种方法制备。
优选的一类无灰分散剂包括用琥珀酸酐基团取代的并与聚亚烷基胺，例如聚亚乙基胺(例如，四亚乙基五胺)，氨基醇例如三羟甲基氨基甲烷和任意的其他反应物例如醇和活性金属例如季戊四醇，和它们的混合物反应的那些无灰分散剂。有效的分散剂还有这样的分散剂，其中通过US3275,554和3,565,804所述的方法(其中卤化烃上的卤素基团用不同的亚烷基聚胺替换)，聚胺直接地连接到主链上。
另一类无灰分散剂包括曼尼希碱缩合产物。通常，例如在US3,442,808中所公开的，通过约1摩尔烷基取代的单-或多羟基苯用约1-2.5摩尔羰基化合物(例如甲醛和低聚甲醛)和约0.5-2摩尔聚亚烷基聚胺缩合而制备的这些产物。这样的曼尼希缩合产物可以包括作为苯基上的取代基的金属茂催化聚合的聚合物，或者可以以类似于US3,442,808所示的方法该缩合物与含有在琥珀酸酐上取代的这种聚合物的化合物反应。
基于使用金属茂催化剂体系合成的官能化和/或衍生的烯烃聚合物的例子描述在上述出版物中。
例如通常在US3087936和3254025中所述，分散剂可以通过各种常规的后处理方法例如硼酸盐化进一步后处理。通过用选自氧化硼，卤化硼，硼酸和硼酸酯的硼化合物处理含酰基氮的分散剂可容易地实现的上述后处理，用量为提供每摩尔酰化氮组合物约0.1原子比例(atomic proportions)的硼至每原子比例酰化氮组合物的氮约20原子比例的硼。有效的分散剂含有约0.05-2.0％(重量)，例如0.05-0.7％(重量)的硼(基于该含硼酸的酰基氮化合物的总重)。我们认为以脱水硼酸聚合物(主要是(HBO2)3)产物形式出现的硼以胺盐例如二酰亚胺的偏硼酸盐的形式与分散剂酰亚胺和二酰亚胺结合。硼酸盐化通过下述方法可容易地进行：将通常是浆液形式的约0.05-4，例如1-3％(重量)(基于酰基氮化合物的重量)的硼化合物，优选硼酸加入到酰基氮化合物中，并在135℃-190℃，例如140℃-170℃下搅拌1-5小时，接着氮汽提。也可以通过将硼酸加入到二羧酸物料和胺的热反应混合物中同时除去水来进行硼处理。
并且，B可以分别地提供，例如以由聚异丁烯琥珀酸酐制备的B酯或B琥珀酰亚胺，其中聚合物的分子量为450-700。
本发明特别有效的组合物是那些含有下述无灰分散剂的组合物，该无灰分散剂是基于数均分子量为900-2500、被已进一步官能化的琥珀酸酐基团取代的聚(异丁烯)聚合物。优选的是，分散剂含有每聚合物基团至少1.0，优选至少1.3个琥珀酸基团。优选的一类官能化化合物含有至少一种NH＜基团。
通常，使用每当量琥珀酸酐取代的聚合物0.5当量-2摩尔胺化合物进行官能化。
其他优选的无灰分散剂是基于上述乙烯α烯烃聚合物的官能化和衍生的烯烃聚合物，该烯烃聚合物是使用金属茂催化剂体系制备的。
油溶性金属清净剂
含金属或灰形成清净剂的作用是作为减少或除去沉积物的清净剂和作为酸中和剂或防锈剂，从而降低磨损和腐蚀并延伸发动机寿命。清净剂通常包括具有长疏水尾基的极性首基，该极性首基含有酸性有机化合物的金属盐。该盐可以含有基本上化学计量的金属，在这种情况下，它们通常被称作正盐或中性盐，并且其总碱值或TBN(例如可用ASTM D2896测定)一般为0-80。通过过量的金属化合物例如氧化物或氢氧化物与酸性气体例如二氧化碳反应可以含有大量的金属碱。得到的高碱性的清净剂含有作为金属碱(例如碳酸盐)胶束外层的中和的清净剂。这样的高碱性的清净剂的TBN可以为150或更大，一般为250-450或更大。
可以使用的清净剂包括油溶性中性和高碱性磺酸盐，酚盐，硫化酚盐，硫代磷酸盐，水杨酸盐，和环烷酸盐和金属特别是碱或碱土金属，例如钠，钾，锂，钙和镁的其他油溶性羧酸盐。最常用的金属是钙和镁，钙和镁都可存在于润滑油中所用的清净剂中，以及钙和/或镁和钠的混合物。特别常规的金属清净剂是具有TBN为20-450的中性和高碱性钙和镁的磺酸盐，和具有TBN为50-450的中性和高碱性钙的酚盐和硫化酚盐。
磺酸盐可由磺酸制备，该磺酸一般通过磺化烷基取代的芳香烃得到，例如由石油分馏得到的或通过芬香烃烷基化得到的那些磺酸。其例子包括通过烷基化苯，甲苯，二甲苯，萘，联苯或他们的卤素衍生物例如氯苯，氯甲苯和氯萘得到的那些。可以在催化剂存在下使用具有约3-多于70个碳原子的烷基化剂进行烷基化。烷芳基磺酸盐的每个烷基取代的芳香族部分含有约9-约80个或更多个碳原子，优选约16-约60个碳原子。
油溶性磺酸盐或烷芳基磺酸可以用金属的氧化物，氢氧化物，醇盐，碳酸盐，羧酸盐，硫化物，氢硫化物，硝酸盐，硼酸盐和醚中和。根据最终产物的所需TBN来选择金属化合物的量，但是该量一般为所需化学计算量的约100-220重量％(优选至少125重量％)。
通过与适当的金属化合物例如氧化物或氢氧化物反应来制备酚和硫化酚的金属盐，并且通过本领域公知的方法可以得到中性或高碱性产物。可通过酚与硫或含硫化合物例如硫化氢、一卤化硫或二卤化硫反应，形成通常是其中两个或多个酚通过含硫桥桥连的化合物的混合物产物来制备硫化酚。
抗磨剂和抗氧化剂
二烃基二硫代磷酸金属盐常用作抗磨剂和抗氧化剂。该金属可以是碱金属或碱土金属，或铝，铅，锡，钼，锰，镍或铜。锌盐最常用于润滑油中，基于润滑油组合物的总重量，锌盐的量为0.1-10，优选0.2-2重量％。该锌盐可按照已知方法制备：通常通过一种或多种醇或酚与P2S5反应先形成二烃基二硫代磷酸(DDPA)，然后用锌化合物中和形成的DDPA。例如，可通过伯醇和仲醇的混合物的反应制备二硫代磷酸。也可以制备多重二硫代磷酸，其中一个烃基在性质上是完全次要的，其他的烃基在性质上是完全主要的。可以使用任何碱性或中性锌化合物来制备锌盐，但是氧化物，氢氧化物和碳酸盐是最常用的。由于在中和反应中使用过量的碱性锌化合物，所以工业添加剂时常含有过量的锌。
优选的二烃基二硫代磷酸锌是二烃基二硫代磷酸的油溶性盐，并可用下列通式表示：
其中R和R′可以是相同的或不同的含有1-18，优选2-12个碳原子的烃基，并包括例如烷基，烯基，芳基，芳基烷基，烷芳基和环脂族的基团。特别优选的R和R′基团是2-8碳原子的烃基。因此，该基团可以是例如乙基，正丙基，异丙基，正丁基，异丁基，仲丁基，戊基，正己基，异己基，正辛基，癸基，十二基，十八基，2-乙基己基，苯基，丁基苯基，环己基，甲基环戊基，丙烯基，丁烯基。为了得到油溶性，在二硫代磷酸中的碳原子(即R和R′)的总数通常将为约5或更大。因此二烃基二硫代磷酸锌可以包括二烷基二硫代磷酸锌。
氧化抑制剂或抗氧化剂减少了矿物油在使用中变质的趋势。氧化变质可以由润滑油中的沉淀物、金属表面上的漆状沉积物和由粘度增大来证实。这样的氧化抑制剂包括受阻酚，优选具有C5～C12烷基侧链的烷基酚硫代酯的碱土金属盐，壬基酚硫化钙，油溶性酚盐和硫化酚盐，磷硫化或硫化烃，亚磷酸酯，金属硫代氨基甲酸盐，在US4,867,890中所述的油溶性铜化合物，和含钼化合物。
具有至少2个直接地连接到氮上的芳基的芳香胺构成了另一类化合物，该类化合物时常用于抗氧化。而这些物料可以少量使用，本发明优选的实施方案没有这些化合物。它们优选只有少量使用，即高达0.4重量％，或更优选除了可以作为杂质从组合物的另一组分产生的这样的量以外应完全避免使用。
通常，具有至少2个直接连接到1个胺氮上的油溶性芳香胺含有6-16个碳原子。该胺可以含有多于2个芳基。下述化合物也认为是具有至少2个直接地连接到氮上的芳基的芳香胺，该化合物总的具有至少3个芳基，其中2个芳基通过1个共价键或通过1个原子或基团(例如，氧或硫原子，或-CO-，-SO2-或亚烷基基团)连接，并且这2个芳基直接地连接到胺氮上。该芳环一般被一个或多个选自烷基，环烷基，烷氧基，芳氧基，酰基，酰氨基，羟基，和硝基的取代基取代。具有至少2个连接到直接地一个胺氮上的芳基的这种油溶性芳香胺的量应优选不超过0.4重量％活性组分。
其他组分
这些组分的例子是金属防锈剂，粘度指数增进剂，防腐剂，其他的抗氧化剂，摩擦改进剂，其他的分散剂，抗泡剂，抗磨添加剂，降凝剂，和防锈剂。有些添加剂在下面进一步详细讨论。
适合的粘度改进剂的代表性例子是聚异丁烯，乙烯和丙烯的共聚物，聚甲基丙烯酸酯，异丁烯酸盐共聚物，不饱和二羧酸和乙烯基化合物的共聚物，苯乙烯和丙烯酸酯的共聚物，和苯乙烯/异戊二烯、苯乙烯/丁二烯、和异戊二烯/丁二烯的部分氢化聚物，以及丁二烯和异戊二烯的部分氢化均聚物。
也可包括与成品油的其他组分相配伍的摩擦改进剂和燃料经济剂(fuel economy agents)。其例子是通过羧酸和酐与链烷醇反应形成的酯，例如高级脂肪酸的甘油基单酯，例如单油酸甘油酯；长链多羧酸与二元醇的酯，例如二聚不饱和脂肪酸的丁二醇酯；噁唑啉化合物；和烷氧基化烷基取代的一元胺，二胺和烷基醚胺，例如乙氧基化牛脂胺和乙氧基化牛脂醚胺。该胺可以这样使用或以与硼化合物例如氧化硼，卤化硼，偏硼酸盐，硼酸或单-，二-或三烷基硼酸盐的加合物或反应产物的形成使用。其他摩擦力改进剂是已知的。其他常规的摩擦力改进剂通常含有共价结合到亲油烃链上的极性端基(例如羧基或羟基)。羧酸和酐与链烷醇的酯描述在US4,702,850中。M.Belzer在“摩擦学杂志(Journal of Tribology)”(1992)，114卷，675-682页，和M.Belzer和S.Jahanmir在“润滑科学(Lubrication Science)”(1988)，1卷，3-26页中描述了其他常规的常规的摩擦力改进剂的例子。
粘度指数增进剂分散剂的功能是既作为粘度指数增进剂又作为分散剂。粘度指数增进剂分散剂的例子包括胺例如聚胺与烃基取代的单-或二羧酸的反应产物，其中该烃基取代基含有向化合物提供粘度指数改善性质的足够长的链。通常，该粘度指数增进剂分散剂可以是，例如乙烯醇或C3-C10不饱和单羧酸或C4-C10二羧酸与不饱和具有4-20个碳原子的含氮单体的C4-C24不饱和酯。C2-C20烯烃与用胺、羟基胺或醇中和的不饱和C3-C10单-或二-羧酸的聚合物；乙烯与C3-C20烯烃的聚合物，该聚合物或者通过将C4-C20不饱和含氮单体接枝到其上或者通过将不饱和酸接枝到聚合物主链上而进一步反应，然后接枝酸的羧酸基团与胺、羟基胺或醇反应。
分散剂和粘度指数增进剂分散剂的的例子可在欧洲专利说明书No.24146B中找到。
降凝剂，也称作润滑油流动改进剂，降低了流体流动或可以倾倒的最低温度。这样的添加剂是公知的。改善流体低温流动性的那些典型添加剂是C8-C18二烷基富马酸/醋酸乙烯酯共聚物，和聚甲基丙烯酸酯。用聚硅氧烷型抗泡剂，例如硅油或聚二甲基硅氧烷可以控制起泡。
胺可以这样使用，也可以以与硼化合物例如氧化硼、卤化硼、偏硼酸盐、硼酸或单-，二-或三烷基硼酸盐的加成物或反应产物的形式使用。其他摩擦力改进剂是已知的。其他常规的摩擦力改进剂通常含有共价结合到亲油烃链上的极性端基(例如羧基或羟基)。羧酸和酐与链烷醇的酯描述在US4,702,850中。在“Journal of Triboiogy”(1992)，114卷，675-682页中的M.Belzer和在“Lubrication Science″(1988)，1卷，3-26页中的M.Belzer和S.描述了其他常规的摩擦力改进剂的例子。
可以使用选自非离子聚氧化亚烷基多元醇及其酯，聚氧化亚烷基酚和阴离子烷基磺酸的防锈剂。
可以使用带有铜和铅的防腐剂。典型的这种化合物是含有5-50个原子的噻二唑(thiadiazole)多硫化物，及其衍生物和聚合物。典型的是1，3，4噻二唑例如描述在US2,719,125；2,719,126；和3,087,932中的那些。其他相似的物质描述在US3,821,236；3,904,537；4,097,387；4,107,059；4,136,043；4,188,299；和4,193,882中。其他添加物是噻二唑的硫代和聚硫代亚磺酰胺，例如描述在UK专利说明书No.1,560,830中的那些化合物。苯并三唑衍生物也落在这类添加剂范围内。
可以使用少量的破乳组分。优先的破乳组分描述在EP330,522中。通过烯化氧与加成物反应得到该破乳组分，所述的加成物通过二-环氧化物与多元醇反应得到。破乳剂的用量为不超过0.1质量％活性组分。适合的处理速度为0.001-0.05质量％活性组分。上述某些添加剂可以提供多重作用；例如单个添加剂可作为分散剂-抗氧化剂。这种方法是已知的，本文不再进一步详细说明。
一般每种添加剂以可使添加剂提供其所需功能的量混入基料油中。
当用于曲轴箱润滑剂时，这种添加剂的代表性的有效量列在下表中。表中列出的所有值是用活性组分质量百分数表示。
添加剂     质量％(宽范围)     质量％(优选)
无灰分散剂     0.1-20     1-8
金属清净剂     0.1-15     0.2-9
防腐剂     0-5     0-1.5
金属二烃基二硫代磷酸盐     0.1-6     0.1-4
抗氧化剂     0-5     0.01-2
降凝剂     0.01-5     0.01-1.5
抗泡剂     0-5     0.001-0.15
补充抗磨剂     0-1.0     0-0.5
摩擦改进剂     0-5     0-1.5
粘度改进剂     0.01-10     0.25-3
基料     余量     余量
本文所表示的所有重量百分数(除非另有说明)是基于添加剂的活性组分(A.I.)的量，和/或添加剂整套配方或配方的总重量，该配方是每个添加剂的活性组分重量和总的油或稀释剂的重量总和。
该组分可以以任何适合的方式加入到基础油中。因此，可以通过将各组分以所需的浓度分散或溶解在油中而将各组分加入到基础油中。各个组分可以是单独的或再混合的。因此，当加入各个清净剂时得到清净剂体系，以致得到了体系的共同特征。这样的混合可以在环境温度或提高的温度下进行。
优选将除了粘度改进剂和降凝剂外的所有的添加物掺入到所述的浓缩液或添加剂整套配方中，然后加入到基料中制成成品润滑油。这种浓缩液的使用是常规的。一般将浓缩液配制成含有适当量的添加剂，所述添加剂的量是当浓缩液与预定量的基础润滑油混合时在最终配方中可提供所需的添加剂浓度。
应当知道，该组合物的各种组分、主要组分以及最佳和常用组分可在配制、贮存或使用的条件下反应，因此，本发明还提供了由任何的这种反应可得到的或得到的产物。
当分散剂和各个清净剂组分可各自地加入到浓缩液时，特别优选的浓缩液是按照US4,938,880所述方法将分散剂与全部清净剂预混合制备的。该专利描述了在至少约100℃的温度下预混合1-10小时制备分散剂和金属清净剂的预混合物，然后冷却预混合物至至少85℃并加入附加组分。
最终配方可使用2-15质量％，优选5-15质量％，一般约10质量％的浓缩液或添加剂整套配方，其余物是基础油。
本发明适用于多种润滑油粘度等级，例如SAE 0W-X，SAE 5W-X和SAE10W-X，其中X是20，30，40或50。
实施例
通过参考下列实施例进一步理解本发明，除非另有说明，其中所有的份数是重量份数，并且这些实施例包括本发明的优选实施方案。
试验方法
所用的方法是VW PV 1449，或T-4试验方法，该方法是在2.0升，2KW，4缸汽油发动机中进行，该方法如下。10小时“试车″和2小时“冲洗(flush)运行”之后，发动机运行试验248小时，包括192小时循环过程和56小时等速运转。在试验过程中不允许“加满”油。试验过程结束时，评定使用过的油的粘度、粘度的增加和总碱值。评定发动机活塞的“环粘着性”和活塞清洁度。
1997年三月的VW 502.00技术规格，中心标准57221描述了润滑油合格的VW的限度。
经验说明粘度增大是一个关键的参数，对于由参考油试验评价该限度为大约130％。
配方试验
由基料，含有无灰分散剂、ZDDP抗氧化剂、含金属清净剂、摩擦改进剂、破乳剂和防泡剂，和单独的粘度改进剂的清净剂防腐剂整套配方(DI整套配方)制备满足AP1 SH/CD技术规格的4个系列SAE 10W-40多等级曲轴箱润滑油，所述的单独的粘度改进剂是具有25SSI的乙烯-丙烯共聚物的油溶液。无灰分散剂是常规的含硼聚异丁烯基琥珀酰亚胺分散剂(PIBSA/PAM)。
4个试验润滑油的不同点主要在于下列聚α烯烃(PAO)的含量：
润滑油            A    1      2     3
PAO含量(质量％)   10   29.9   45    50
因为改变了PAO含量所以也要调节矿物油含量和粘度改进剂的处理量。
用上述VW PV 1449方法试验这4个润滑油。
试验结果
在发动机试验结束时得到这些润滑油的粘度增大值：
润滑油         A      1      2      3
粘度增大(％)   301    190    103    64.5
用于润滑油的PAO是具有100℃下的标称粘度为6cSt的聚α烯烃。润滑油A是对比润滑油，润滑油1，2和3是本发明润滑油。
因此可以看出，通过增加基料中PAO的比例至润滑油2和3任意地满足VW PV 1449方法的所需粘度增大的要求，可使粘度增大明显地变小。

Claims (11)

1.一种用于内燃机的润滑油组合物，含有：
(A)主要量的润滑粘度基料，该基料含有从45％到小于70质量％的一种或多种按API 1509定义的具有粘度为100℃下2-20mm2s-1的IV类基料或其混合物，和
(B)两种或多种添加剂组分，包括一种或多种无灰分散剂和一种或多种金属清净剂。
2.根据权利要求1的组合物，其中基料含有45-68质量％的所述一种或多种IV类基料。
3.根据权利要求1的组合物，其中IV类基料是具有2-16个碳原子的支链或直链α烯烃的低聚物。
4.根据权利要求1的组合物，其中其余的基料是一种或多种按API1509定义的I类基料。
5.根据权利要求1的组合物，其中一种或多种无灰分散剂包括含有用琥珀酸酐取代的和与聚亚烷基胺反应的聚合烃主链的分散剂。
6.根据权利要求1或5的组合物，其中金属清净剂是钙或镁的油溶性中性或高碱性磺酸盐、酚盐或水杨酸盐。
7.一种制备润滑油组合物的方法，包括混合(A)和(B)，每个(A)和(B)与上述任一项权利要求的定义相同。
8.权利要求1-6之任一项的润滑油组合物或权利要求7的方法制备的润滑油组合物在润滑内燃机的发动机中的用途。
9.根据权利要求8的用途，其中发动机是点燃式发动机。
10.权利要求1-6之任一项的润滑油组合物或权利要求7的方法制备的润滑油组合物在提高点燃式发动机中曲轴箱润滑油更换周期的处理发动机的运动表面中的用途。
11.含25到80质量％的一种或多种按API 1509定义的IV类基料的润滑粘度基料在改进VW PV 1449或T-4试验中的性能中的用途。
CN98808718A 1997-08-01 1998-07-23 润滑油组合物 Expired - Lifetime CN1117839C (zh)

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