CN1880420B - 具有低发烟量的低灰或无灰双循环润滑油 - Google Patents
具有低发烟量的低灰或无灰双循环润滑油 Download PDFInfo
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- CN1880420B CN1880420B CN2006100918606A CN200610091860A CN1880420B CN 1880420 B CN1880420 B CN 1880420B CN 2006100918606 A CN2006100918606 A CN 2006100918606A CN 200610091860 A CN200610091860 A CN 200610091860A CN 1880420 B CN1880420 B CN 1880420B
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Abstract
本发明公开了一种新的低烟双循环油，其包含高反应性聚异丁烯(“HR-PIB”)、溶剂添加剂包，并且在100℃下的运动粘度为至少6.5mm2/s，JASO M342烟指数为至少85。该新的双循环油是由可有效地替代常规双循环油中传统包含的聚异丁烯(“PIB”)的替代性原料制得的。
Description
技术领域
本发明涉及一种用作双循环油的润滑油组合物。更具体地，本发明涉及双循环油，其特征在于它是无灰的，或包含较低量的金属清净剂，但符合针对地上设备、汽油作为燃料的双循环发动机，例如摩托车发动机、摩托自行车发动机、雪上汽车发动机、割草机发动机等的特定发烟测试标准和粘度要求。
背景技术
如今，双冲程循环汽油发动机较小的有低于50cc的发动机，较高性能发动机超过了500cc。这种高性能发动机的发展产生了对新的双循环油标准和测试过程的需要。
传统的双循环发动机是通过混合燃料和润滑油，并使混合的组合物通过发动机来进行润滑的。较新的双循环发动机可能涉及直接使用燃料注射以减少排放。在上述两种情况下，油通过发动机并燃烧。各种与燃料相容的双循环油在本领域中已有描述。通常，这种油含有各种添加剂组分，以使该油通过工业标准测试，从而获准用在双循环发动机中。
全球范围的对燃料经济性和环境清洁性的要求已激励双循环油的制造商要满足对粘度和发烟量的日益严格的标准。在许多情况下，这些新标准常规上通过使用更大量的昂贵原料以制造新的改进的双循环油来得以满足。因此，存在一种对满足燃料经济性和环境清洁性新标准的可替代原料的需求。
发明内容
本发明基于这样的发现：使用特定比例的高反应性聚异丁烯聚合物、溶剂和润滑油基础料以及适量的双循环润滑油添加剂包(package)，可以提供具有合适粘度性质的低灰或无灰双循环发动机油，该油可超过JASO(日本汽车标准组织)M342烟指数测试。高反应性聚-丁烯聚合物(也称为HR-PIB)与传统的聚-丁烯(称为PIB)相比包含更多的末端亚乙烯基双键，并且由不同的制备工艺制得。含HR-PIB的双循环油是传统双循环油的有用且有效的替代品。
一方面，本发明是低灰双循环润滑油组合物，其在100℃下的运动粘度为至少6.5mm2/s(cSt)，JASO M342烟指数为至少85。该组合物包含：
(a)15-35wt％的选自聚丁烯、聚异丁烯或聚丁烯和聚异丁烯的混合物的烯键式不饱和聚合物，其数均分子量为400-2200，且其末端亚乙烯基含量基于该聚合物中双键总数为至少60mol％；
(b)20-30wt％的通常呈液态的烃或矿物油溶剂，其在25℃下的粘度为1-5cP；
(c)1-5wt％的用于双循环油的添加剂包；和
(d)矿物油或合成油或其混合物，其在100℃下的粘度为4-15mm2/s(cSt)。
另一方面，本发明是无灰双循环润滑油组合物，其在100℃下的运动粘度为至少6.5mm2/s(cSt)，JASO M342烟指数为至少85。该组合物包含：
(a)6-12wt％的反应性聚丁烯聚合物，其为聚丁烯、聚异丁烯或聚丁烯和聚异丁烯的混合物，其数均分子量为400-2200，且具有至少60mol％的作为末端亚乙烯基的双键；
(b)18-30wt％的通常呈液态的烃或矿物油溶，其在25℃下的粘度为1-5cP；
(c)14-25wt％的用于双循环油的不含金属的添加剂包；和
(d)余量的矿物油或合成油或其混合物，其在100℃下的粘度为4-15mm2/s(cSt)。
具体实施方式
本发明中使用的高反应性聚丁烯聚合物(下文中称“HR-PIB”)包括聚丁烯、聚异丁烯或其混合物，其Mn为400-2200，优选约800-1500，例如约1000，其末端亚乙烯基含量基于双键总摩尔数为至少60mol％。末端亚乙烯基含量优选为至少70％，更优选至少80％，最优选至少85％。通过引用将下列已公开专利的全部内容，特别是关于高反应性聚异丁烯制备方法的教导结合于此：美国专利No.4152499、No.5962604、No.6562913、No.6683138和No.6710140。HR-PIB的其它来源有可商购的商用名(BASF)和
(BP-Amoco)等。
本发明使用的溶剂通常为液态的天然烃或合成烃或矿物油溶剂，其在25℃下的粘度为1-5cP，优选1.2-2cP。该溶剂的闪点应为约60-120℃，以使本发明的双循环油的闪点高于70℃。典型的例子包括链烷烃、异链烷烃和脂族环烷烃或矿物油溶剂。该溶剂可以包含除碳和氢以外的官能团，只要这些基团不对双循环油的性能产生负面影响。矿物油优选是ExxonMobil Chemical Company出售的“Exxsol D80”和Shell Chemicals出售的“Shellsol D70”。
本发明还可包含添加剂包作为第三组分：对于低灰油，含有1-5wt％；对于无灰油，含有14-25wt％，该添加剂包含有一种或多种常规的双循环润滑油添加剂，并且它们可以是这种润滑油中通常包含的用于特定目的的任何添加剂。对于无灰包，其中基本不合金属添加剂。
用于本发明的添加剂包组分的常规添加剂包括抗蚀剂、氧化抑制剂、摩擦改进剂、分散剂、防沫剂、抗磨剂、倾点降低剂、金属清净剂、防锈剂、润滑剂等。所有百分比都基于活性成分的重量。
优选的低灰添加剂包包含(i)聚异丁烯(Mn为400-2500，优选约950)琥珀酰亚胺或另一种油溶性酰化含氮润滑油分散剂，其存在量为润滑油的0.2-5wt％，优选1-3wt％，和(ii)金属酚盐、磺酸盐或水杨酸盐油溶性清净添加剂。此清净剂是中性金属清净剂或总碱值为200或更低的高碱性金属清净剂，其存在量为润滑油的0.1-2wt％，优选0.2-1wt％。金属优选为钙、钡或镁。中性水杨酸钙是优选的，其存在量可以为润滑油的约0.5-1.5wt％。
优选的无灰添加剂包包含在油中约5.5-17wt％、优选9-15wt％的无灰润滑油分散剂，而且可以使用一种或多种如下所公开的无灰分散剂。
本发明使用的分散剂包括含氮无灰分散剂，已知当该分散剂添加到润滑油中时可有效地减少在汽油和柴油发动机中使用后沉淀的形成。这些无灰分散剂具有含能与待分散粒子结合的官能团的油溶性聚合长链骨架。通常，胺、胺醇或酰胺极性部分一般通过桥基与聚合物骨架连接。无灰分散剂例如可以选自长链烃取代的一元和多元羧酸或其酸酐的油溶性盐、酯、氨基酯、酰胺、酰亚胺和唑啉；长链烃的硫代羧酸盐衍生物；具有与其直接相连的聚胺部分的长链脂族烃；和通过缩合长链取代的酚与甲醛和聚亚烷基多胺形成的曼尼希缩合产物。
可用于制备分散剂的聚异丁烯聚合物一般是基于约400-3000道尔顿的烃链。制备聚异丁烯的方法是众所周知的。如下所述，可以通过卤化(例如氯化)、经热“烯化”反应(“ene”reaction)的热反应或通过使用催化剂(例如过氧化物)的自由基接枝而使聚异丁烯官能化。
官能化的油溶性聚合烃骨架也可以与例如一元醇和多元醇的羟基化合物衍生，或与例如苯酚和萘酚的芳族化合物衍生。优选的多元醇包括亚烷基二醇，其中亚烷基包含2-8个碳原子。其它可用的多元醇包括甘油、甘油的单油酸酯、甘油的单硬脂酸酯、甘油的单甲基醚、季戊四醇、二季戊四醇及其混合物。酯类分散剂也可以衍生自不饱和醇，例如烯丙醇、肉桂醇、炔丙醇、1-环己烷-3-醇和油醇。其它类的能生成无灰分散剂的醇还包括醚-醇，包含氧-亚烷基和氧-亚芳基。这些醚-醇可以包含至多150个氧-亚烷基，其中亚烷基具有1-8个碳原子。酯类分散剂可以是琥珀酸的二酯或酸酯，例如部分酯化的琥珀酸，以及部分酯化的多元醇或酚，例如具有游离醇或酚羟基的酯。可以通过例如美国专利No.3381022中所述的几种已知方法中的任意一种来制备酯类分散剂。
如上所述，优选类别的分散剂包括Mn为400-2200的高反应性聚异丁烯的琥珀酰亚胺。这些分散剂通常通过将聚异丁烯琥珀酸酐与例如三亚乙基四胺或四亚乙基五胺的亚烷基聚胺反应来制备。
另一类高分子量无灰分散剂包括曼尼希碱缩合产物。通常，这些产物通过缩合约1摩尔长链烷基取代的单或多羟基苯与约1-2.5摩尔羰基化合物(例如，甲醛和低聚甲醛)和约0.5-2摩尔聚亚烷基多胺来制备，例如美国专利No.3442808中所述的。
油中存在的抗蚀剂的量可以为0.01-3wt％，优选0.01-1.5wt％，其例子有磷硫化烃和通过将磷硫化烃与碱土金属氧化物或氢氧化物反应而得到的产物。
油中存在的氧化抑制剂的量可以为0.01-5wt％，优选0.01-1.5wt％。合适的氧化抑制剂包括优选具有C5-C12烷基侧链的烷基酚硫醚的碱土金属盐，例如壬基酚硫化钙、叔辛基酚硫化钡，以及二辛基酚胺。氧化抑制剂还包括油溶性硫化或磷硫化烃和抗氧化性铜化合物，例如C10-C18油溶性脂肪酸的铜盐。
油中存在的摩擦改进剂的量可以为0.01-3wt％，优选0.01-1.5wt％，其包括脂肪酸酯和酰胺、二聚脂肪酸的甘油酯和琥珀酸酯或其金属盐。
油中存在的倾点抑制剂(也称为润滑油流动改进剂)的量可以为0.01-2wt％，优选0.01-1.5wt％。合适的倾点抑制剂是优选的富马酸的C8-C18或C14二烷基酯醋酸乙烯酯共聚物、聚甲基丙烯酸酯和蜡搽(wax naphthalene)。
还可以通过防沫剂提供泡沫控制。防沫剂可以是聚硅氧烷类，例如硅油和聚二甲基硅氧烷；丙烯酸酯聚合物也是合适的。油中使用的防沫剂的量为0.01-5wt％，优选0.01-1.5wt％。
抗磨剂减少金属部分的磨损，其代表性材料为二烷基二硫代磷酸锌、二芳基二磷酸锌和硫化异丁烯。油中使用的抗磨剂的量为0.01-5wt％。
本发明所用的润滑剂包括各种油溶性材料。油中使用的润滑剂的量一般为1-20wt％，优选1-7wt％。润滑剂包括多元醇醚和多元醇酯，例如C5-C15一元羧酸的多元醇酯，特别是这些酸的季戊四醇、三羟甲基丙烷和新戊二醇合成润滑油(synlube)酯，其中该酯在100℃下的粘度至少为9mm2/s(cSt)；天然油例如光亮油是优选的，它是由石油制备润滑油馏分时形成的蒸馏残余物衍生得到的高粘性矿物油馏分。
本发明的润滑组合物通常包含具有润滑粘度(即在100℃下为约4-15，优选12-15mm2/s(cSt)的粘度)的油，以提供在100℃下的运动粘度为6.5-14mm2/s(cSt)的成品双循环油。
这些具有润滑粘度的油可以是天然油或合成油。这种油的混合物也经常有用。也可以使用油的混合物，只要该混合物在100℃下的最终粘度为4-15mm2/s(cSt)。
天然油包括优选的矿物润滑油，例如链烷烃类、环烷烃类或链烷烃-环烷烃混合类的液态石油和溶剂处理或酸处理的矿物润滑油。源自煤或页岩的具有润滑粘度的油也是有用的基础油。
合成润滑油包括烃类油，例如聚合和共聚的烯烃，烷基化二苯基醚和烷基化二苯基硫醚及其衍生物、类似物和同系物。
通过少于5个碳原子的烯烃及其混合物的聚合制得的油是典型的合成聚合物油。制备这些聚合物油的方法对于本领域的技术人员是公如的，如在例如美国专利No.2278445、No.2301052、No.2318719、No.2329714、No.2345574和No.2422443中所示的。
环氧烷聚合物(例如，均聚物、共聚物及其衍生物，其中末端羟基已通过酯化、醚化等修饰)是用于本发明目的的一类优选的已知合成润滑油，特别是与链烷醇燃料组合使用。其例子为通过聚合环氧乙烷或环氧丙烷制备的油、这些聚氧亚烷基聚合物的烷基或芳基醚(例如，平均分子量为1000的甲基聚丙二醇醚、分子量为500-1000的聚乙二醇的二苯基醚、分子量为1000-1500的聚丙二醇二乙基醚等)或其一元和多元羧酸酯，例如醋酸酯混合的C3-C8脂肪酸酯，或四甘醇的C13含氧酸二酯。
另一类合适的合成润滑油包括二羧酸(例如，苯二甲酸、琥珀酸、烷基琥珀酸、链烯基琥珀酸、马来酸、壬二酸、辛二酸、癸二酸、富马酸、己二酸、亚油酸二聚体、丙二酸、烷基丙二酸、链烯基丙二酸等)与各种链烷醇(例如，丁醇、己醇、辛醇、十二烷醇、十三烷醇、2-乙基己醇、乙二醇、二甘醇单醚、丙二醇等)的酯。这些酯的具体例子包括己二酸二辛酯、癸二酸二(2-乙基己基)酯、富马酸二正己酯、癸二酸二辛酯、壬二酸二异辛酯、壬二酸二异癸酯、邻苯二甲酸二辛酯、邻苯二甲酸二癸酯、癸二酸二廿烷基酯、亚油酸二聚体的2-乙基己基二酯、由1摩尔癸二酸与2摩尔四甘醇和2摩尔2-乙基己酸反应所形成的复合酯等。优选的酯在100℃下的粘度为5-12mm2/s(cSt)。
可作为合成油使用的酯还包括那些由C5-C18一元羧酸和多元醇和多元醇醚(例如新戊二醇、三羟甲基丙烷、季戊四醇、二季戊四醇、三季戊四醇等)制备的酯。
本发明的润滑油组合物中可以使用以上公开类型的末精制的、精制的和再精制的天然油或合成油(以及它们中的两种或更多种的混合物)。未精制的油是那些直接从天然源或合成源得到的未经进一步纯化处理的油。例如，直接从干馏操作得到的页岩油、直接从初级蒸馏得到的石油或直接从酯化工艺得到的酯油、并且未经进一步处理而使用的是未精制油。精制油与未精制油类似，不同之处在于精制油在一个或多个纯化步骤中被进一步处理以改善一种或多种性质。许多这样的纯化技术对本领域的技术人员而言是已知的，例如溶剂萃取、次级蒸馏、酸或碱萃取、过滤、渗滤等。再精制油是通过那些与用来获得已经采用的精制油的类似工艺而得到的。这样的再精制油也称为再生油或再处理油，并且经常通过涉及去除已消耗的添加剂和油分解产物的相关技术而被额外处理。
本发明的润滑油组合物可以与这种双循环发动机中所用的燃料自由混合。该润滑油与燃料的混合物构成了本发明的另一实施方案。双循环发动机中使用的燃料对本领域的技术人员是公知的，并且通常包含主更部分的通常为液态的燃料，例如烃类石油馏分燃料，例如根据ASTM规范D-439-73定义的摩托车汽油。这样的燃料还可以包含非烃类物质，例如醇、醚、有机硝基化合物等。例如，甲醇、乙醇、二乙醚、甲乙醚、硝基甲烷以及这样的燃料，如从植物和矿物源(例如玉米、α页岩和煤)获得的液体燃料在本发明的范围内。这样的燃料混合物的例子是汽油与乙醇、柴油燃料与乙醚、汽油与硝基甲烷的组合等。汽油是优选的。汽油指ASTM沸点为60℃(10％蒸馏点)至约205℃(90％蒸馏点)的烃混合物。无铅汽油是特别优选的。
本发明的润滑油在与燃料的混合物中的用量为每1重量份润滑油约20-250重量份燃料，更常见地每1重量份油约30-100重量份燃料。
通过以下实施例进一步举例说明本发明。这些实施例旨在更好地表达本发明而无意以任何方式限制本发明的范围。百分比为重量百分比。
实施例
根据JASO M345测试过程JASO M340、M341、M342和M343，评价含反应性HR-PIB的本发明的油(在下表中以“本发明”表示)和含常规聚异丁烯的常规油(在下表中以“常规”表示)。这些是日本汽车工程师协会(JSAE)针对双循环汽油发动机油而建立的发动机测试。从1994年7月1日起，依据日本汽车标准组织(JASO)宣布的JASO-M345标准对在双循环发动机中使用的油进行标识。JASO于1994年4月公布了JASO M345标准，并于2004年予以更新。“EGD清净性”是对常规JASO M341清净性测试过程(1小时)的进一步改进，其中EGD测试进行3小时。这是已被ISO(国际标准化组织)采用的更严格标准。“FC”是更新之前JASO M345标准的最高性能标准。2004年的更新版本引入了“FD”分类，类似于ISO-EGD。此测试的结果示于下表中。
表
| 质量百分比 | 本发明 | 常规 |
| 低灰添加剂包 | 2.25 | 2.25 |
| PIB(聚异丁烯，Mn950) | 0 | 25.00 |
| HR-PIB(Glissopal1000，Mn1000) | 25.00 | 0 |
| 脂族溶剂(Shellsol D70) | 25.00 | 25.00 |
| 矿物油(Shell HVI 160B) | 47.50 | 47.50 |
| 结果 |
| 100℃下的运动粘度，cSt(JASO≥6.5) | 7.25 | 7.30 |
| M342烟指数(JASO FD/FC/ISO-EGD≥85) | 89 | 88 |
表中数据表明，含HR-PIB的低灰双循环油的粘度和烟指数性能实际上与包含相应量PIB的常规低灰二冲程油的相同。因此，此数据表明HR-PIB可用来替代PIB配制和制造低灰二冲程油。
Claims (6)
1. 一种低灰双循环润滑油组合物，其在100℃下的运动粘度为至少6.5mm2/s(cSt)，JASO M342烟指数为至少85，所述组合物包含：
(a)15-35wt％的选自聚-烯、聚异丁烯或聚丁烯和聚异丁烯的混合物的烯键式不饱和聚合物，其数均分子量为400-2200，末端亚乙烯基含量基于聚合物中双键总数为至少60mol％；
(b)20-30wt％的通常呈液态的烃或矿物油溶剂，其在25℃下的粘度为1-5cP；
(c)1-5wt％的用于双循环油的添加剂包；和
(d)矿物油或合成油，或其混合物，其在100℃下的粘度为4-15mm2/s(cSt)。
2. 一种无灰双循环润滑油组合物，其在100℃下的运动粘度为至少6.5mm2/s(cSt)，JASO M342烟指数为至少85，所述组合物包含：
(a)6-12wt％的选自聚丁烯、聚异丁烯或聚丁烯和聚异丁烯的混合物的烯键式不饱和聚合物，其数均分子量为400-2200，末端亚乙烯基含量基于聚合物中双键总数为至少60mol％；
(b)18-30wt％的通常为液态的烃或矿物油溶剂，其在25℃下的粘度为1-5cP；
(c)14-25wt％的用于双循环油的不含金属的添加剂包；和
(d)矿物油或合成油，或其混合物，其在100℃下的粘度为4-15mm2/s(cSt)。
3. 如权利要求1或2的组合物，其中所述烯键式不饱和聚合物是Mn为800-1500的高反应性聚丁烯。
4. 如权利要求1或2的组合物，其中所述溶剂在25℃下的粘度为1.2-2cP。
5. 如权利要求1或2的组合物，其中所述矿物油或合成油或其混合物在100℃下的粘度为12-15mm2/s(cSt)。
6. 如权利要求1或2的组合物，其中所述添加剂包包含由高反应性聚异丁烯聚合物制备的琥珀酰亚胺分散剂。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11/153,723 US20060287202A1 (en) | 2005-06-15 | 2005-06-15 | Low ash or ashless two-cycle lubricating oil with reduced smoke generation |
| US11/153,723 | 2005-06-15 |
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| CN1880420A CN1880420A (zh) | 2006-12-20 |
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| US (1) | US20060287202A1 (zh) |
| EP (1) | EP1743932A3 (zh) |
| JP (1) | JP2006348297A (zh) |
| CN (1) | CN1880420B (zh) |
| AU (1) | AU2006202573B2 (zh) |
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| JP5173289B2 (ja) * | 2007-07-06 | 2013-04-03 | 出光興産株式会社 | ２サイクルエンジン用潤滑油組成物 |
| US20090062161A1 (en) * | 2007-08-27 | 2009-03-05 | Joseph Timar | Two-cycle gasoline engine lubricant |
| ATE542842T1 (de) * | 2009-12-21 | 2012-02-15 | Infineum Int Ltd | Polymer und polymerzusammensetzungen |
| JP5959622B2 (ja) * | 2011-05-04 | 2016-08-02 | ザ ルブリゾル コーポレイションＴｈｅ Ｌｕｂｒｉｚｏｌ Ｃｏｒｐｏｒａｔｉｏｎ | オートバイのエンジン用潤滑剤 |
| RU2013153814A (ru) | 2011-05-05 | 2015-06-10 | Шелл Интернэшнл Рисерч Маатсхаппий Б.В. | Композиции смазочного масла, содержащие базовые масла, полученные способом фишера-тропша |
| WO2016138939A1 (en) | 2015-03-03 | 2016-09-09 | Basf Se | Pib as high viscosity lubricant base stock |
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- 2006-06-15 SG SG201006655-3A patent/SG166094A1/en unknown
- 2006-06-15 AU AU2006202573A patent/AU2006202573B2/en not_active Ceased
- 2006-06-15 JP JP2006165796A patent/JP2006348297A/ja active Pending
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| Publication number | Publication date |
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| JP2006348297A (ja) | 2006-12-28 |
| SG128610A1 (en) | 2007-01-30 |
| EP1743932A3 (en) | 2007-09-05 |
| CN1880420A (zh) | 2006-12-20 |
| EP1743932A2 (en) | 2007-01-17 |
| US20060287202A1 (en) | 2006-12-21 |
| AU2006202573A1 (en) | 2007-01-11 |
| AU2006202573B2 (en) | 2011-11-03 |
| SG166094A1 (en) | 2010-11-29 |
| CA2550562C (en) | 2011-07-05 |
| CA2550562A1 (en) | 2006-12-15 |
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