CN103717719A - 包含聚(异丁烯)/聚(乙烯基芳烃)嵌段共聚物的润滑组合物 - Google Patents
包含聚(异丁烯)/聚(乙烯基芳烃)嵌段共聚物的润滑组合物 Download PDFInfo
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- CN103717719A CN103717719A CN201280036305.7A CN201280036305A CN103717719A CN 103717719 A CN103717719 A CN 103717719A CN 201280036305 A CN201280036305 A CN 201280036305A CN 103717719 A CN103717719 A CN 103717719A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
- C10M143/10—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing aromatic monomer, e.g. styrene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
- C08F293/005—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule using free radical "living" or "controlled" polymerisation, e.g. using a complexing agent
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M143/00—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2438/00—Living radical polymerisation
- C08F2438/01—Atom Transfer Radical Polymerization [ATRP] or reverse ATRP
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/026—Butene
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2205/00—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions
- C10M2205/04—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing aromatic monomers, e.g. styrene
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2020/00—Specified physical or chemical properties or characteristics, i.e. function, of component of lubricating compositions
- C10N2020/01—Physico-chemical properties
- C10N2020/04—Molecular weight; Molecular weight distribution
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2030/00—Specified physical or chemical properties which is improved by the additive characterising the lubricating composition, e.g. multifunctional additives
- C10N2030/04—Detergent property or dispersant property
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
- C10N2040/00—Specified use or application for which the lubricating composition is intended
- C10N2040/04—Oil-bath; Gear-boxes; Automatic transmissions; Traction drives
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Abstract
本发明提供一种润滑组合物，所述润滑组合物包含具有润滑粘度的油和聚(烯烃)嵌段如聚(异丁烯)(PIB)与聚(乙烯基芳烃)嵌段如聚(苯乙烯)的嵌段共聚物，其中共聚物为任选官能化或接枝的。本发明进一步提供使用该嵌段共聚物控制润滑油组合物中的沉积物的方法。
Description
发明领域
本发明涉及润滑组合物，特别是包含具有润滑粘度的油和具有聚(烯烃)嵌段与聚(乙烯基芳烃)嵌段的嵌段共聚物的润滑组合物。
发明背景
聚合物在具有润滑粘度的油中作为粘度改进剂或分散剂粘度改进剂(也称为VM)的用途是熟知的。好的VM会对环境温度有反应以提供所需水平的粘度改进。差执行的VM会导致例如在低温下粘度的不理想提高和/或当分解时不理想的效应。例如，在高温，例如活塞筒中发现的那些下，粘度改进剂的无效降解会导致降解物燃烧和筒中的碳形成。远离高温，无效的降解可导致粘度改进剂的氧化，导致不理想的粘度提高。
特别是对于烯烃共聚物粘度改进剂，例如乙烯-丙烯共聚物(OCP)，在发动机活塞沉积物方面通常观察到有限的洁净度。尽管OCP提供良好的低温性能，但OCP具有氧化倾向，而且在高温下无效地降解。
与OCP相反，聚(乙烯基芳烃)聚合物(PVA聚合物)，例如聚(苯乙烯)有效得多地降解，但是是油不溶的。油溶性可通过与二烯如丁二烯共聚而赋予PVA聚合物，例如苯乙烯。事实上，研究了苯乙烯丁二烯共聚物作为粘度改进剂或分散剂粘度改进剂，显示与主线乙烯-丙烯共聚物相比活塞沉积物方面的改善。例如，美国公开No.2010/0152082公开了通过阴离子聚合而产生的苯乙烯-丁二烯嵌段共聚物。然而，二烯不会有效的降解，并且需要例如通过加入羰基侧基而官能化。
已知聚(异丁烯)(PIB)不会氧化并且在高温下会有效地降解。然而，PIB不具有良好的增稠性能并且显示出差的低温性能。
能够用作VM的共聚物并可提供可接受的低温性能和/或清洁度中的至少一项并且可简单地制备的共聚物是理想的。
发明概述
现在发现乙烯基芳烃如苯乙烯与异丁烯的共聚物提供良好的VM性能和优越的降解性能。因而，本发明提供用于润滑组合物中的聚(乙烯基芳烃)-聚(异丁烯)(PVA-PIB)嵌段共聚物，例如聚(苯乙烯)-聚(异丁烯)(PS-PIB)。
在一个实施方案中，本发明提供包含具有润滑粘度的油和PVA-PIB嵌段共聚物的润滑组合物。PVA-PIB嵌段共聚物可以是或者不是递变嵌段共聚物，并且由至少一个PIB嵌段(嵌段A)和至少一个PVA嵌段(嵌段B)组成，其中嵌段A/(嵌段A+B)的摩尔比为0.5-0.97。在一个实施方案中，嵌段B的PVA可以为聚(苯乙烯)(PS)。如本文所用，短语“嵌段A/(嵌段A+B)的摩尔比”意指嵌段A中的重复单元的摩尔数除以(嵌段A+嵌段B)中的重复单元之和的比。重复单元指聚合物中的单体衍生单元。
在一个实施方案中，本发明提供具有润滑粘度的油、如本文所公开的PVA-PIB共聚物和至少一种添加剂的润滑组合物，所述添加剂包括分散剂、抗氧化剂、抗磨剂、摩擦改进剂或其混合物。
在一个实施方案中，润滑组合物包含具有润滑粘度的油、如本文所公开的PS-PIB共聚物和分散剂或其混合物。
在一个实施方案中，润滑组合物包含具有润滑粘度的油、如本文所公开的PVA-PIB共聚物和抗氧化剂或其混合物。
在一个实施方案中，润滑组合物包含具有润滑粘度的油、如本文所公开的PVA-PIB共聚物和抗磨剂或其混合物。
在一个实施方案中，润滑组合物包含具有润滑粘度的油、如本文所公开的PVA-PIB共聚物和摩擦改进剂或其混合物。
在一个实施方案中，对内燃机而言，如本文所述润滑剂组合物具有降低量的硫、磷和硫酸盐灰中的至少一种。
在一个实施方案中，本发明提供润滑组合物在用于2冲程或4冲程内燃机的发动机油、齿轮油、自动变速器油、水力流体、涡轮机油、金属加工流体或循环油中的用途。
发明详述
本发明提供用于润滑组合物中的PVA聚合物与PIB的嵌段共聚物。本发明共聚物包括PIB的嵌段“A”和PVA的嵌段“B”。
尽管嵌段B PVA可基于具体应用的要求选择，在一个实施方案中，嵌段B的PVA可包含苯乙烯单体。PVA也可由取代的苯乙烯如甲基苯乙烯、α-卤代苯乙烯、低级烷基取代的苯乙烯如α-甲基苯乙烯、α-乙基苯乙烯、对-叔丁基苯乙烯和对-低级烷氧基苯乙烯组成。二官能乙烯基芳族单体如二乙烯苯也可以以少量存在。二-(和更高)官能单体可用于制备交联和星形聚合物，并且可以以聚合物组成物的至多5%使用。在一个实施方案中，聚合物不含(或基本不含)多官能乙烯基芳族单体。
嵌段A PIB可完全解聚，同时赋予嵌段B油溶性。嵌段B PVA可赋予润滑配制剂剪切稳定性、良好的低温性能和增稠并且理想地完全解聚。因此，存在于共聚物中的嵌段A和嵌段B的量可基于润滑流体的需要而减少。优选嵌段A/(嵌段A+B)的摩尔比为0.5-0.97，但也可以为0.7-0.95，或0.75-0.9。如本文所用，短语“嵌段A/(嵌段A+B)的摩尔比”意指嵌段A中的重复单元的摩尔数除以(嵌段A+嵌段B)中的重复单元之和的比。
在本发明各个实施方案中，嵌段聚合物的结构可以为线性、支化或星形的，并且嵌段可以以规则、无规则、顺序、递变或交替顺序排列。嵌段共聚物可以为二嵌段AB共聚物，或者三嵌段ABA或BAB共聚物。在一个实施方案中，共聚物可以为线性规则共聚物。在另一实施方案中，共聚物可以为二嵌段序列嵌段共聚物或二嵌段星型共聚物。如本文所用，术语“序列嵌段共聚物”意指由离散嵌段(A和B)组成的共聚物，所述嵌段各自为均相的，即由单一单体构成。序列嵌段共聚物的实例包括A-B或B-A-B结构的那些。
在一些实施方案中，本发明PIB嵌段可包含少量二烯。关于共聚物中嵌段A的含量，二烯内容物可以以小于10摩尔%，或小于5摩尔%，或小于2摩尔%存在。合适的二烯包括例如1,4-丁二烯或异戊二烯。在一些实施方案中，嵌段A可基本不含或甚至完全不含二烯。如本文所用，术语“基本不含二烯”意指聚合物含有不多于杂质含量，通常为聚合物的小于1摩尔%，或者聚合物的0.05摩尔%或更少，或者聚合物的0.01摩尔%或更少，或者聚合物的0摩尔%的二烯衍生单元。当嵌段共聚物包含二烯时，二烯可以为支化或线性的，且共聚物以为氢化或未氢化的。
在一个实施方案中，可将嵌段A的异丁烯单体和嵌段B的乙烯基芳族单体中的一个或者两者用基团，包括酰基或卤素-、烷氧基-、羧基-、羟基-、磺酰基-、硝基-、亚硝基-和烃基取代基官能化，其中烃基通常具有1-12个碳原子。
在另一实施方案中，可将嵌段A的异丁烯单体和嵌段B的乙烯基芳族单体中的一个或者两者用烯键式不饱和酰化剂接枝。接枝可通过将PVA-PIB骨架上的乙烯基碳卤化(例如溴化)，然后使卤化的乙烯基碳与羧酸或其衍生物在活化剂的存在下反应而进行，如例如2011年1月13日公开的WO/2011/005739，Price等人中所教导的。
可将酰化聚合物用胺或多胺进一步官能化。在一个实施方案中，由于碳形成控制或燃料经济性，胺包含芳族胺。在一个实施方案中，由于可接受的碳形成和/或淤渣处理，胺可以为脂族胺。
共聚物的重均分子量可以为1000-1,000,000，或5,000-500,000，或10,000-250,000，或50,000-175,000。在不同的实施方案中，共聚物的多分散性通常为1至小于1.6，或1-1.55，或1-1.4，或1.01-1.2。
本发明共聚物可以以本领域技术人员已知的任何方式制备。例如，如例如Principles of Polymerization，George Odian，第3版，第356页所教导的活性阳离子聚合可提供得到相对于其它方法具有相对高量的乙烯基芳烃衍生单元如苯乙烯的产物的快速且可定制路线。可提供以可控方式将新的官能引入PIB嵌段中的方法的另一技术可以为ATRP聚合，例如如Handbook of Radical Polymerization，Krzysztof Matyjaszewski编辑，第523页所教导的，ATRP聚合可提供具有较低量的乙烯基芳烃衍生单元的共聚物。发明人发现通过使用不同的方法制备PIB-PVA嵌段共聚物，可控制共聚物的PVA含量，由此提供具有差异化分解度的嵌段共聚物。
具有润滑粘度的油
组合物包含具有润滑粘度的油。这类油包括天然和合成油、衍生自加氢裂化、氢化和加氢精制的油，未精炼、精炼和再精炼油及其混合物。
未精炼油为通常不经(或经很少的)进一步提纯处理，直接由天然或合成来源得到的那些。精炼油类似于未精炼油，不同的是已将它们在一个或多个提纯步骤中进一步处理以改善一种或多种性能。提纯技术为本领域中已知的，包括溶剂萃取、二次蒸馏、酸或碱萃取、过滤、渗滤等。
再精炼油也称作再生或再加工油，通过类似于用于得到精炼油的方法得到并通常另外通过旨在除去废添加剂和油分解产物的技术加工。
用于制备本发明润滑剂的天然油包括动物油、植物油(例如蓖麻油、猪油)、矿物润滑油如液体石油或者链烷烃、环烷烃或混合链烷烃-环烷烃型的溶剂处理或酸处理的矿物润滑油，和衍生自煤或页岩的油，或其混合物。
合成润滑油是有用的，包括烃油，例如聚合和共聚烯烃(例如聚丁烯、聚丙烯、丙烯异丁烯共聚物)；聚(1-己烯)、聚(1-辛烯)、聚(1-癸烯)及其混合物；烷基苯(例如十二烷基苯、十四烷基苯、二壬基苯、二-(2-乙基己基)苯)；聚苯(例如联苯、三联苯、烷基化聚苯)；烷基化二苯醚和烷基化二苯硫及其衍生物、类似物和同系物或其混合物。
其它合成润滑油包括含磷酸的液体酯(例如磷酸三甲苯酯、磷酸三辛酯和癸烷膦酸的二乙基酯)，和聚四氢呋喃。合成油可通过费托反应制备，通常可以为加氢异构化的费托合成烃或蜡。在一个实施方案中，油可通过费托天然气合成油(gas-to-liquid)合成程序制备以及其它天然气合成油。
具有润滑粘度的油也可如American Petroleum Institute(API)BaseOil Interchangeability Guidelines所述定义。五组基油如下：组I(硫含量>0.03重量%，和/或<90重量%饱和物，粘度指数80-120)；组II(硫含量≤0.03重量%，且≥90重量%饱和物，粘度指数80-120)；组III(硫含量≤0.03重量%，且≥90重量%饱和物，粘度指数≥120)；组IV(所有聚α烯烃(PAO))；和组V(所有不包括在组I、II、III或IV中的其它基油)。具有润滑粘度的油包括API组I、组II、组III、组IV、组V油或其混合物。通常，具有润滑粘度的油为API组I、组II、组III、组IV油或其混合物。或者，具有润滑粘度的油通常为API组I、组II、组III油或其混合物。
润滑剂组合物可以为浓缩物和/或完全配制润滑剂的形式。如果本发明聚合物为浓缩物的形式(其可与其它油组合形成全部或部分最终润滑剂)，则聚合物与具有润滑粘度的油和/或与稀释油的重量比为1:99-99:1，或80:20-10:90。
其它性能添加剂
组合物任选包含其它性能添加剂。其它性能添加剂包括如下至少一种：金属减活剂、常规清净剂(通过本领域已知方法制备的清净剂)、分散剂、粘度改进剂、摩擦改进剂、抗磨剂、腐蚀抑制剂、分散剂粘度改进剂、特压剂、抗磨擦剂、抗氧化剂、抑泡剂、反乳化剂、倾点下降剂、密封溶胀剂及其混合物。通常，完全配制润滑油含一种或多种这些性能添加剂。
分散剂
分散剂通常已知为无灰型分散剂，因为在混入润滑油组合物中以前，它们不含有成灰金属且当加入润滑剂和聚合分散剂中时它们通常不会贡献任何成灰金属。无灰型分散剂特征在于通过连接在较高分子量烃链上的极性基团。典型的无灰分散剂包括N-取代的长链链烯基琥珀酰亚胺。N-取代的长链链烯基琥珀酰亚胺的实例包括PIB取代基的数均分子量为350-5000，或500-3000的PIB琥珀酰亚胺。琥珀酰亚胺分散剂和它们的制备方法例如公开于美国专利4,234,435中。琥珀酰亚胺分散剂通常为由多胺，通常聚(乙烯胺)或芳族多胺如氨基二苯胺(ADPA)形成的酰亚胺。
在一个实施方案中，本发明还包含至少一种PIB琥珀酰亚胺分散剂，所述分散剂衍生自数均分子量为350-5000，或500-3000的PIB。PIB琥珀酰亚胺可以单独或与其它分散剂组合使用。
在一个实施方案中，本发明还包含至少一种衍生自PIB琥珀酸酐、胺和氧化锌以形成与锌的PIB琥珀酰亚胺配合物的分散剂。与锌的PIB琥珀酰亚胺配合物可以单独或组合使用。
另一类无灰分散剂为曼尼希碱。曼尼希分散剂为烷基苯酚与醛(尤其是甲醛)和胺(尤其是聚亚烷基多胺)的反应产物。烷基通常含至少30个碳原子。
也可将分散剂通过常规方法通过与多种试剂中任一种反应而后处理。其中，这些为硼、脲、硫脲、二巯基噻二唑、二硫化碳、醛、酮、羧酸、烃取代的琥珀酸酐、马来酸酐、腈、环氧化物、磷化合物和/或金属化合物。
分散剂可以以润滑组合物的0-20重量%，或0.1-15重量%，或0.1-10重量%，或1-6重量%，或7-12重量%存在。
清净剂
润滑剂组合物任选还包含其它已知的中性或高碱性清净剂。合适的清净剂基质包括酚盐、含硫酚盐、磺酸盐、salixarate、水杨酸盐、羧酸、磷酸、单-和/或二硫代磷酸、烷基酚、硫耦合的烷基酚化合物，或水杨苷。各种高碱性清净剂和它们的制备方法更详细地描述于大量专利出版物，包括WO2004/096957和其中引用的参考文献中。
清净剂可以以0-10重量%，或0.1-8重量%，或1-4重量%，或大于4至8重量%存在。
抗氧化剂
抗氧化剂化合物是已知的，包括例如硫化烯烃、二芳基胺、受阻酚、钼化合物(例如二硫代氨基甲酸钼)及其混合物。抗氧化剂化合物可以单独使用或组合使用。抗氧化剂可以以润滑组合物的0-20重量%，或0.1-10重量%，或1-5重量%，在一些情况下1.5-3.0重量%存在。
受阻酚抗氧化剂通常含有仲丁基和/或叔丁基作为空间位阻基团。酚基可以进一步被烃基和/或连接在第二个芳基上的桥联基团取代。合适的受阻酚抗氧化剂的实例包括2,6-二叔丁基苯酚、4-甲基-2,6-二叔丁基苯酚、4-乙基-2,6-二叔丁基苯酚、4-丙基-2,6-二叔丁基苯酚或4-丁基-2,6-二叔丁基苯酚或4-十二烷基-2,6-二叔丁基苯酚。在一个实施方案中，受阻酚抗氧化剂可以为酯，可包括例如来自Ciba的IrganoxTML-135。合适的含酯受阻酚抗氧化剂化学的更详细描述在美国专利6,559,105中找到。
二芳基胺抗氧化剂可含有一个或多个氮原子。芳基可在两个氮原子之间或者一个氮原子可具有两个连接于其上的芳基。二芳基胺抗氧化剂中芳基的取代基可包括脂族烃基如具有1-30个碳原子的烷基、羟基、卤素基团、羧酸或酯基团或硝基。优选芳基可以为取代或未取代的苯基或萘基。一个或两个芳基可以被取代，例如单烷基化二苯胺、二烷基化二苯胺，或单-和二-烷基化二苯胺的混合物。可使用的二芳基胺的合适实例包括但不限于二苯胺和烷基化二苯胺、苯基萘胺和烷基化苯基-萘胺及其混合物。
可用作抗氧化剂的二硫代氨基甲酸钼的合适实例包括以商品名如Molyvan822TM和MolyvanTMA由R.T.Vanderbilt Co.，Ltd.和以AdekaSakura-LubeTMS-100、S-165和S-600由Asahi Denka Kogyo K.K出售的商业材料及其混合物。
粘度改进剂
尽管本发明聚合物可用作粘度改进剂，也可存在其它类型的其它粘度改进剂。这类粘度改进剂是熟知的材料，包括氢化的苯乙烯-丁二烯橡胶、乙烯-丙烯共聚物、氢化的苯乙烯-异戊二烯聚合物、氢化的异戊二烯聚合物、聚(甲基)丙烯酸酯(通常聚甲基丙烯酸烷基酯)、聚烷基苯乙烯、聚烯烃和马来酸酐-苯乙烯共聚物的酯，或其混合物。这类其它粘度改进剂可以以润滑组合物的0-15重量%，或0.1-10重量%，或1-5重量%，或在一些情况下0.5-2重量%存在。
抗磨剂
润滑剂组合物任选还包含至少一种其它抗磨剂。抗磨剂可以以润滑组合物的0-15重量%，或0.1-10重量%或1-8重量%，或在一些情况下0.5-2重量%存在。合适抗磨剂的实例包括磷酸酯，硫化烯烃，含硫无灰抗磨添加剂，为金属二烃基二硫代磷酸盐(例如二烷基二硫代磷酸锌)，含硫代氨基甲酸酯的化合物，例如硫代氨基甲酸酯、硫代氨基甲酸酯酰胺、硫代氨基甲酸醚、亚烷基耦合的硫代氨基甲酸酯和双(S-烷基二硫代氨甲酰基)二硫化物。
含二硫代氨基甲酸酯的化合物可通过使二硫代氨基甲酸或盐与不饱和化合物反应而制备。含二硫代氨基甲酸酯的化合物也可通过使胺、二硫化碳和不饱和化合物同时反应而制备。一般而言，反应在25-125℃的温度下进行。美国专利4,758,362和4,997,969描述了二硫代氨基甲酸酯化合物及其制备方法。
可硫化以形成硫化烯烃的合适烯烃的实例包括丙烯、丁烯、异丁烯、戊烯、己烷、庚烯、辛烷、壬烯、癸烯、十一碳烯、十二碳烯、十一烷基、十三碳烯、十四碳烯、十五碳烯、十六碳烯、十七碳烯、十八烯、十八碳烯、十九碳烯、二十碳烯或其混合物。在一个实施方案中，十六碳烯、十七碳烯、十八烯、十八碳烯、十九碳烯、二十碳烯或其混合物和它们的二聚物、三聚物和四聚物是尤其有用的烯烃。或者，烯烃可以为二烯如1,3-丁二烯和不饱和酯如丙烯酸丁酯的第尔斯阿尔德(Diesl-Alder)加成物。
另一类硫化烯烃包括脂肪酸和它们的酯。脂肪酸通常由植物油或动物油得到，通常含4-22个碳原子。合适脂肪酸和它们的酯的实例包括甘油三酯、油酸、亚油酸、棕榈油酸或其混合物。通常，脂肪酸由猪油、妥尔油、花生油、豆油、棉子油、向日葵子油或其混合物得到。在一个实施方案中，将脂肪酸和/或酯与烯烃混合。
在可选实施方案中，无灰抗磨剂可以为多元醇与脂族羧酸，通常含有12-24个碳原子的酸的单酯。通常，多元醇与脂族羧酸的单酯为与向日葵油等的混合物的形式，其可以以所述混合物的5-95，或在其它实施方案中10-90，或20-85，或20-80重量%存在于摩擦改进剂混合物中。形成酯的脂族羧酸(尤其是单羧酸)为通常含有12-24或14-20个碳原子的那些酸。羧酸的实例包括十二烷酸、硬脂酸、月桂酸、山萮酸和油酸。
多元醇包括二元醇、三乙醇和具有更高数目的醇类OH基团的醇。多元醇包括乙二醇，包括二甘醇、三甘醇和四甘醇；丙二醇，包括二丙二醇、三丙二醇和四丙二醇；甘油；丁二醇；己二醇；山梨糖醇；阿糖醇；甘露糖醇；蔗糖；果糖；葡萄糖；环己二醇；赤藓醇；和季戊四醇，包括二季戊四醇和三季戊四醇。通常，多元醇为二甘醇、三甘醇、甘油、山梨糖醇、季戊四醇或二季戊四醇。
称为“单油酸甘油酯”的市售单酯被认为包含60±5重量%化学物种单油酸甘油酯，以及35±5%二油酸甘油酯和小于5%三油酸酯和油酸。上述单酯的量基于存在任何这类混合物中的多元醇单酯的实际校正量计算。
抗磨蚀剂
润滑剂组合物还可包含抗磨蚀剂。认为降低粘附磨损的抗磨蚀剂化合物通常为含硫化合物。通常，含硫化合物包括有机硫化物和聚硫化物，例如二苄基二硫醚、双(氯苄基)二硫硫化物、二丁基四硫化物、二-叔丁基聚硫化物、油酸的硫化甲酯、硫化烷基苯酚、硫化二戊烯、硫化萜烯、硫化迪尔斯阿尔德加合物、烷基亚氧硫基N’N-二烷基二硫代氨基甲酸酯、多胺与多元酸酯的反应产物、2,3-二溴丙氧基异丁酸的氯代丁酯、二烷基二硫代氨基甲酸的乙酰氧基甲酯和黄原酸的酰氧基烷基醚及其混合物。
特压剂
可溶于油中的特压剂(EP)包括含硫和含氯硫的EP剂、氯化烃EP剂和磷EP剂。这类EP剂的实例包括氯化蜡；有机硫化物和聚硫化物，例如二苄基二硫化物、双-(氯苄基)二硫化物、二丁基四硫化物、硫化的油酸甲酯、硫化烷基酚、硫化二戊烯、硫化萜烯和硫化第尔斯阿尔德加成物；磷硫化烃，例如硫化磷与松节油或油酸甲酯的反应产物；磷酯，例如二烃和三烃亚磷酸酯，例如亚磷酸二丁酯、亚磷酸二庚酯、亚磷酸二环己酯、亚磷酸戊基苯酯；亚磷酸二戊基苯酯、亚磷酸十三烷基酯、亚磷酸二硬脂基酯和聚丙烯取代的苯酚亚磷酸酯；金属硫代氨基甲酸盐，例如二辛基二硫代氨基甲酸锌和庚基苯酚二酸钡；二硫代磷酸的锌盐；烷基和二烷基磷酸的胺盐，包括例如二烷基二硫代磷酸与氧化丙烯的反应产物的胺盐；及其混合物。
其它添加剂
其它性能添加剂如腐蚀抑制剂包括美国申请US05/038319(2004年10月25日提交，指定发明人McAtee和Boyer)第5-8段所述那些、辛胺辛酸盐、十二碳烯基琥珀酸或酐和脂肪酸如油酸与多胺的缩合产物。在一个实施方案中，腐蚀抑制剂包括腐蚀抑制剂。Synalox腐蚀抑制剂通常为氧化丙烯的均聚物或共聚物。
腐蚀抑制剂更详细地描述于Dow Chemical Company出版的产品手册Form No.118-01453-0702AMS中。该产品手册标题为“SYNALOX Lubricants，High-PerformancePolyglycols for Demanding Applications”。
金属减活剂，包括苯并三唑的衍生物、二巯基噻二唑衍生物、1,2,4-三唑、苯并咪唑、2-烷基二硫代苯并咪唑或2-烷基二硫代苯并噻唑；抑泡剂，包括丙烯酸乙酯和丙烯酸2-乙基己酯和任选乙酸乙烯酯的共聚物；反乳化剂，包括磷酸三烷基酯、聚乙二醇、聚氧化乙烯、聚氧化丙烯和(氧化乙烯-氧化丙烯)聚合物；倾点下降剂，包括马来酸酐-苯乙烯的酯、聚甲基丙烯酸酯、聚丙烯酸酯或聚丙烯酰胺；和摩擦改进剂，包括脂肪烷基组分，例如脂肪酸衍生物，例如胺、酯、环氧化物、脂肪咪唑啉、羧酸与聚亚烷基多胺的缩合产物，和烷基磷酸的胺盐也可用于润滑剂组合物中。脂肪烷基通常意指C10-C22烷基，其通常为直链且任选不饱和的。摩擦改进剂可以以润滑组合物的0-10重量%或0.1-8重量%或1-5重量%存在。
工业应用
本发明共聚物适于任何润滑剂组合物。聚合物可用作粘度改进剂和/或分散剂粘度改进剂(通常称为DVM)。
在一个实施方案中，本发明聚合物提供如下至少一种性能：可接受的粘度改进性能、可接受的分散剂性能和可接受的碳堆积和淤渣处理。当本发明聚合物用于发动机油润滑剂组合物中时，它通常进一步提供可接受的燃料经济性能或可接受的碳堆积和淤渣处理。
润滑剂的实例包括用于2冲程或4冲程内燃机的发动机油、齿轮油、自动变速器油、水力流体、涡轮机油、金属加工流体或循环油。
在一个实施方案中，内燃机可以为柴油燃烧发动机、汽油燃烧发动机、天然气燃烧发动机或混合汽油/醇燃烧发动机。在一个实施方案中，内燃机为柴油燃烧发动机，在另一实施方案中，为汽油燃烧发动机。
内燃机可以为2冲程或4冲程发动机。合适的内燃机包括船用柴油机、航空用活塞发动机、低负荷柴油机，以及汽车和卡车发动机。
用于内燃机的润滑剂组合物可适于任何发动机润滑剂而不管硫、磷或硫酸盐灰(ASTM D-874)含量。发动机油润滑剂的硫含量可以为0.01-1重量%，或0.01-0.8重量%，或0.01-0.5重量%，或0.01-0.3重量%。同样，发动机油可不具有任何硫含量。发动机油的磷含量可以为0.01-0.2重量%，或0.01-0.1重量%，或0.01-0.085重量%，或甚至0.01-0.06重量%，或0.01-0.055重量%，或0.01-0.05重量%。同样，发动机油可不包含任何磷。总硫酸盐灰含量可以为0.01-2重量%，或0.01-1.5重量%，或0.01-1.1重量%，或0.01-1重量%，或0.01-0.8重量%，或0.01-0.5重量%。同样，发动机油可不含，或者基本不含任何硫酸盐灰含量。
在一个实施方案中，润滑组合物为发动机油，其中润滑组合物具有(i)0.5重量%或更少的硫含量，(ii)0.1重量%或更少的磷含量，和(iii)1.5重量%或更少的硫酸盐灰含量。
在一个实施方案中，润滑组合物适于2冲程或4冲程船用柴油内燃机。在一个实施方案中，船用柴油燃机为2冲程发动机。可将本发明聚合物以0.01-20重量%，或0.05-10重量%，或0.1-5重量%加入船用柴油润滑组合物中。
在几个实施方案中，合适的润滑组合物包含基于活性物质以表1a和1b所示范围存在的添加剂。
表1a
表1b
以下实施例提供对本发明的阐述。这些实施例不是详尽的且不意欲限制本发明的内容。
实施例
实施例1-活性阳离子聚合
PS-PIB共聚物根据下面的反应式通过活性阳离子聚合用异丙苯基氯引发剂和TiCl4促进剂制备。所得共聚物具有约19.4摩尔%苯乙烯和80.6摩尔%异丁烯、13900的Mw、11200的Mn和1.23的多分散性。
实施例2–ATRP聚合
PS-PIB共聚物根据下面的示意式通过硼氢化转化成ATRP大分子引发剂，最后转化成苯乙烯-b-异丁烯而由高亚乙烯基5000Mn PIB制备。所得共聚物具有约4.7摩尔%苯乙烯和95.3摩尔%异丁烯、10600的Mw和8600的Mn。
实施例3–热解重量分析(TGA)
为确定PS-PIB共聚物的热分解的类型、速率和程度，使用TGA以相对于PIB(Mw37,000，约40-50%高反应性PIB)、苯乙烯-丁二烯橡胶(SBR)(Mw130,000，约29摩尔%苯乙烯)和OCP(Mw130,000)试样，对比根据实施例1和2的方法制备的产物。
方法：(1)在氮气中热分解—Hi.Res.Sensitivity1.0，以10℃/min上升，达到5-550℃，切换成空气，以10℃/min上升，达到5-600℃，(2)在285℃下恒温—以30℃/min上升至285℃，切换成空气，恒温1440分钟。
结果：(1)基于保留1-4%聚合物时的温度(表1)，两种PS-PIB产物(等级2和3)都显示出接近PIB(等级1)的性能。两种PS-PIB共聚物都比OCP(等级5)和SBR(等级4)执行得好得多。借助ATRP路线合成的PS-PIB(等级2)是比借助活性阳离子聚合合成的共聚物(等级3)更好的执行者。基于无机残余物(表2)，本发明共聚物评级为2和并列为4。通常已知PIB完全分解，推测ATRP共聚物的较低苯乙烯含量是与活性阳离子共聚物性能差别的原因。
(2)设计等温实验以模拟在涡轮增压直接喷油式(TDI)发动机的第2活塞环棱(land ring)温度时聚合物的行为。如表3中所见，最好的执行者也是PIB，其后非常接近的是两种本发明共聚物。较低苯乙烯含量的ATRP共聚物也是比活性阳离子共聚物更好的执行者。
如本说明书中所用，术语“烃基取代基”或“烃基”以其本领域技术人员熟知的常用意义使用。具体而言，它指具有直接连接在分子其余部分上的碳原子且主要具有烃性质的基团。烃基的实例包括：
(i)烃取代基，即脂族(例如烷基或链烯基)、脂环族(例如环烷基、环烯基)取代基，和芳族-、脂族-和脂环族取代的芳族取代基，以及其中环通过该分子的另一部分完成(例如两个取代基一起形成环)的环状取代基；
(ii)取代的烃取代基，即含有在本发明上下文中不改变取代基的主要烃性质的非烃基团(例如卤素(尤其是氯和氟)、羟基、烷氧基、巯基、烷基巯基、硝基、亚硝基和亚硫酰基)的取代基；
(iii)杂取代基，即在本发明上下文中，在具有主要烃性质的同时在由碳原子组成的环或链中含有不同于碳的取代基。杂原子包括硫、氧和氮，且包括取代基如吡啶基、呋喃基、噻吩基和咪唑基。一般而言，对于每10个碳原子，在烃基中存在不多于2，优选不多于1个非烃取代基；通常，烃基中不存在非烃取代基。
已知一些上述材料在最终配制剂中可能相互作用，使得最终配制剂的组分可能与起初加入的那些不同。由此形成的产品，包括经以其意欲用途使用本发明润滑剂组合物而形成的产品可能不容易描述。然而，所有这类改进和反应产物均包括在本发明的范围内；本发明包括通过将上述组分混合而制备的润滑剂组合物。
通过引用将以上提及的各文件结合到本文中。除实施例中或另外明确说明外，在本说明书中描述材料的量、反应条件、分子量、碳原子数等的所有数量应当理解被措辞“约”修饰。除非另有说明，本文提及的各个化学品或组合物应当理解为可含有异构体、副产物、衍生物和通常应当理解存在于商品级中的其它这类材料的商品级材料。然而，除非另有说明，各个化学组分的量表示为排除了通常可存在于商业材料中的任何溶剂或稀释油。应当理解本文所述量、范围和比的上限和下限可独立地组合。类似地，本发明各个元素的范围和量可以与任何其它元素的范围或量一起使用。
尽管已关于优选实施方案解释了本发明，应当理解经阅读本说明书，其各个改进会为本领域技术人员所了解。因此，应当理解此处公开的发明意欲涵盖属于所附权利要求书范围内的这类改进。
Claims (16)
1.一种润滑组合物，其包含：具有润滑粘度的油，和包含至少一个聚(异丁烯)(PIB)聚合物嵌段(嵌段A)和至少一个聚(乙烯基芳烃)(PVA)聚合物嵌段(嵌段B)的嵌段共聚物，其中嵌段A/(嵌段A+B)的摩尔比为0.5-0.97。
2.根据权利要求1的组合物，其中PVA为聚(苯乙烯)(PS)。
3.根据权利要求1的组合物，其中嵌段A/(嵌段A+B)的摩尔比为约0.96。
4.根据权利要求1的组合物，其中嵌段A/(嵌段A+B)的摩尔比为约0.80。
5.根据权利要求1的组合物，其中嵌段A包含小于10摩尔%的二烯衍生单元。
6.根据权利要求1的润滑组合物，其中嵌段共聚物借助活性阳离子聚合制备。
7.根据权利要求1的润滑组合物，其中嵌段共聚物为借助活性阳离子聚合和ATRP聚合制备的嵌段共聚物的混合物。
8.根据权利要求1的润滑组合物，其中嵌段共聚物借助ATRP聚合制备。
9.根据权利要求1的润滑组合物，其中共聚物具有1000-1,000,000的数均分子量。
10.根据权利要求9的润滑组合物，其中共聚物具有10,000-250,000的数均分子量。
11.根据权利要求1的润滑组合物，其中氢化共聚物具有1至小于1.6的多分散性。
12.根据权利要求11的润滑组合物，其中氢化共聚物具有1.01-1.4的多分散性。
13.根据权利要求1的润滑组合物，其中共聚物为二嵌段共聚物。
14.根据权利要求1的润滑组合物，其中共聚物为序列嵌段共聚物。
15.一种控制润滑剂组合物中的沉积物的方法，其包括向润滑剂组合物中加入包含至少一个PIB聚合物嵌段(嵌段A)和至少一个PVA聚合物嵌段(嵌段B)的嵌段共聚物，其中嵌段A/(嵌段A+B)的摩尔比为0.5-0.97。
16.根据权利要求15的方法，其中PVA聚合物为聚(苯乙烯)。
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| US61/489,305 | 2011-05-24 | ||
| PCT/US2012/038750 WO2012162207A1 (en) | 2011-05-24 | 2012-05-21 | Lubricating composition comprising poly (isobutylene) /poly (vinyl aromatic) block copolymer |
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| CN111247179A (zh) * | 2017-10-14 | 2020-06-05 | Tpc集团有限责任公司 | 非无规异丁烯共聚物 |
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| WO2019040576A1 (en) * | 2017-08-25 | 2019-02-28 | Exxonmobil Research And Engineering Company | ASH-FREE LUBRICANTS FOR ENGINES FOR HIGH TEMPERATURE APPLICATIONS |
| WO2020126494A1 (en) | 2018-12-19 | 2020-06-25 | Evonik Operations Gmbh | Use of associative triblockcopolymers as viscosity index improvers |
| EP4179049A1 (en) * | 2020-07-09 | 2023-05-17 | ExxonMobil Technology and Engineering Company | Engine oil lubricant compositions and methods for making same with superior engine wear protection and corrosion protection |
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| US3992310A (en) * | 1971-11-16 | 1976-11-16 | The British Petroleum Company Limited | Copolymers |
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| US3976607A (en) | 1968-05-10 | 1976-08-24 | Velsicol Chemical Corporation | Copolymers and preparational method therefor |
| US3948868A (en) | 1969-04-03 | 1976-04-06 | Exxon Research And Engineering Company | Homogeneous styrene/isoolefin copolymers |
| GB1360689A (en) * | 1971-11-16 | 1974-07-17 | British Petroleum Co | Polystyrene/polyisobutylene vi improver |
| US3994993A (en) | 1975-06-19 | 1976-11-30 | The Firestone Tire & Rubber Company | Diblock copolymers and process of preparing same |
| US4234435A (en) | 1979-02-23 | 1980-11-18 | The Lubrizol Corporation | Novel carboxylic acid acylating agents, derivatives thereof, concentrate and lubricant compositions containing the same, and processes for their preparation |
| US4758362A (en) | 1986-03-18 | 1988-07-19 | The Lubrizol Corporation | Carbamate additives for low phosphorus or phosphorus free lubricating compositions |
| US4997969A (en) | 1988-12-12 | 1991-03-05 | The Lubrizol Corporation | Carbamate additives for lubricating compositions |
| US5038319A (en) | 1989-04-24 | 1991-08-06 | Xerox Corporation | System for recording and remotely accessing operating data in a reproduction machine |
| US5458796A (en) * | 1994-03-31 | 1995-10-17 | Shell Oil Company | Synthesis of polyisobutylene star-branched polymers via living carbocationic polymerization |
| US7056983B2 (en) * | 1998-04-28 | 2006-06-06 | Kaneka Corporation | Block copolymer |
| US6265486B1 (en) | 1998-12-31 | 2001-07-24 | Exxon Mobil Chemical Patents Inc. | Triblock copolymers incorporating a styrene/isoolefin copolymer midblock |
| US6228945B1 (en) * | 1999-12-20 | 2001-05-08 | The University Of Akron | Three arm star compositions of matter having diblock arms based on polyisobutylene and methods of preparation |
| US6559105B2 (en) | 2000-04-03 | 2003-05-06 | The Lubrizol Corporation | Lubricant compositions containing ester-substituted hindered phenol antioxidants |
| WO2004096957A1 (en) | 2003-04-24 | 2004-11-11 | The Lubrizol Corporation | Diesel lubricant low in sulfur and phosphorus |
| JP2009531531A (ja) * | 2006-03-27 | 2009-09-03 | ザ ルブリゾル コーポレイション | ポリマーおよびその潤滑組成物 |
| CA2652555A1 (en) * | 2006-05-17 | 2007-11-29 | The University Of Akron | Method of purifying block copolymers |
| JP5203590B2 (ja) | 2006-10-27 | 2013-06-05 | 出光興産株式会社 | 潤滑油組成物 |
| US8778854B2 (en) | 2009-07-08 | 2014-07-15 | The Lubrizol Corporation | Dispersant viscosity modifiers |
| JP2012219243A (ja) * | 2011-04-13 | 2012-11-12 | Kaneka Corp | 潤滑油用粘度指数向上剤および液体潤滑油組成物 |
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| US3992310A (en) * | 1971-11-16 | 1976-11-16 | The British Petroleum Company Limited | Copolymers |
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| CN111247179A (zh) * | 2017-10-14 | 2020-06-05 | Tpc集团有限责任公司 | 非无规异丁烯共聚物 |
| CN111247179B (zh) * | 2017-10-14 | 2023-08-25 | Tpc集团有限责任公司 | 非无规异丁烯共聚物 |
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| WO2012162207A1 (en) | 2012-11-29 |
| JP2014517865A (ja) | 2014-07-24 |
| CN103717719B (zh) | 2016-06-15 |
| EP2714870A1 (en) | 2014-04-09 |
| US20140274850A1 (en) | 2014-09-18 |
| JP5917685B2 (ja) | 2016-05-18 |
| US9428709B2 (en) | 2016-08-30 |
| CA2837056A1 (en) | 2012-11-29 |
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