CN103354832B - 含有粘度指数改进剂的润滑剂组合物 - Google Patents
含有粘度指数改进剂的润滑剂组合物 Download PDFInfo
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- CN103354832B CN103354832B CN201180067197.5A CN201180067197A CN103354832B CN 103354832 B CN103354832 B CN 103354832B CN 201180067197 A CN201180067197 A CN 201180067197A CN 103354832 B CN103354832 B CN 103354832B
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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
- C10M143/06—Lubricating compositions characterised by the additive being a macromolecular hydrocarbon or such hydrocarbon modified by oxidation containing 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
- C10M161/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a non-macromolecular compound, each of these compounds being essential
-
- 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
- C10M165/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound and a compound of unknown or incompletely defined constitution, each of these compounds being essential
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Abstract
本发明涉及含有聚合物形式的粘度指数改进剂的润滑剂组合物，所述聚合物包含衍生自乙烯、丙烯和丁烯的结构单元。
Description
技术领域
本发明涉及含有粘度指数(VI)改进剂的润滑剂组合物。更特别地，本发明涉及含有聚合物形式的VI改进剂的润滑剂组合物，所述聚合物包含衍生自乙烯、丙烯和丁烯的结构单元。
背景
石油产品通常随着温度变化显示出大的粘度变化。然而，对于用于汽车等的润滑油组合物，优选粘度的温度相关性是小的。为降低粘度的温度相关性，将烯烃共聚物作为VI改进剂加入润滑油组合物中。
概述
多年来，乙烯-丙烯共聚物在多级发动机油配制剂中用作VI改进剂。在多数情况下，这些VI改进剂含有至少约40重量%乙烯。尽管这些共聚物为有效的VI改进剂，当油经受高温操作时，它们具有贡献活塞沉积物和油增稠的缺点。本发明通过该问题的解决方法。
本发明涉及含有VI改进剂的润滑剂组合物，所述VI改进剂包含具有衍生自乙烯、丙烯和丁烯的结构单元的聚合物。当发动机在高温条件下操作时，这些润滑剂组合物在用作发动机油时显示出与常规润滑剂组合物相比降低的活塞沉积物水平和降低的粘度增加水平。本发明涉及润滑剂组合物，其包含：具有润滑粘度的油；和粘度指数改进量的聚合物，所述聚合物包含约5至约20摩尔%衍生自乙烯的结构单元、约50摩尔%或60至约90摩尔%衍生自丙烯的结构单元和约5至约30摩尔%衍生自丁烯的结构单元。在某些实施方案中，润滑剂组合物进一步包含分散剂和包含过碱性磺酸盐的清净剂，其中磺酸盐具有约250至约600的总碱值。
详述
说明书和权利要求书中所述所有范围和比值的极限可以以任何方式组合。应当理解除非另外具体指出，提及“一个/一种”和/或“该”可包括一种或多于一种，且提及单数项，还可包括复数项。
当指连接在分子的其余部分上的基团时，术语“烃基”和“烃”指在本发明上下文内纯粹具有烃性质或主要具有烃性质的基团。这类基团包括：
(1)纯粹烃基团；即脂族、脂环族、芳族、脂族-和脂环族取代的芳族、芳族取代的脂族和脂环族基团等，以及其中环通过分子的另一部分完成的环状基团(即任何两个所述取代基可一起形成脂环族基团)。实例包括甲基、辛基、环己基、苯基等。
(2)取代的烃基；即含有不改变基团的主要烃性质的非烃取代基的基团。实例包括羟基、硝基、氰基、烷氧基、酰基等。
(3)杂基团；即在主要具有烃性质时，在若非如此由碳原子组成的链或环中含有不同于碳的原子的基团。实例包括氮、氧和硫。
通常烃基或烃基团中对于每10个碳原子存在不多于约3个、并且在一个实施方案中存在不多于1个取代基或杂原子。
在本文中与术语如烃基、烷基、链烯基、烷氧基等一起使用的“低级”意欲描述含有总计至多7个碳原子的这类基团。
术语“油溶性”指在25°C下在矿物油中可溶解至至少约0.5g/l的程度的材料。
术语“TBN”指总碱值。这是中和所有或一部分材料碱度所需酸(高氯酸或氢氯酸)的量，作为mgKOH/g试样表示。除非另外指出，通常报告TBN而不就油或可存在于材料中的其它稀释剂的量校正，并以这种方式用于本文件中。
术语“TAN”指总酸值。这是中和所有或一部分材料酸度所需碱(NaOH或KOH)的量，作为mgKOH/g试样表示。
润滑剂组合物
润滑组合物可以由一种或多种基油组成，所述基油可以以主要量存在。基油可以以大于约60重量%，或大于约70%，或大于约75重量%的润滑剂组合物存在。
润滑剂组合物可具有在100°C下至多约26.1cSt，或在100°C下约5.6至约26.1cSt，或在100°C下约6至约16.3cSt，或在100°C下约6至约13cSt的粘度。
润滑剂组合物可具有0W-20、0W-30、0W-40、0W-50、0W-60、5W-20、5W-30、5W-40、5W-50、5W-60、10W-20、10W-30、10W-40、10W-50、15W-20、15W-30、15W-40、15W-50或15W-60的SAE粘度等级。
具有润滑粘度的油
具有润滑粘度的油可称为基油。基油可选自如AmericanPetroleumInstitute(API)BaseOilInterchangeabilityGuidelines所述组I-V中的任一种基油。五组基油如下：
基油可含有小于约300ppm硫和/或至少约90%饱和物含量，通过ASTMD2007所述试验程序测定。基油可具有至少约95，或至少约115的粘度指数。基油可具有至少约120的粘度指数，并且包含一种或多种聚α烯烃。在某些实施方案中，基油可具有至多约130的粘度指数。在某些实施方案中，具有润滑粘度的油可包含组II油。在某些实施方案中，润滑剂组合物内具有润滑粘度的油可总体上具有一定量的组II油，或者组III油，即使总基油可通过将多种各组油混合而制备。
组I、II和III为矿物油基本油料。基油可包含天然或合成润滑油及其混合物。可使用矿物油和合成油，特别是聚α烯烃和酯油的混合物。
天然油包括动物油和植物油(例如蓖麻油、猪油和其它植物酸酯)以及矿物润滑油，例如液体石油油料，和烷烃、环烷烃或混合烷烃-环烷烃型的溶剂处理或酸处理矿物润滑油。加氢处理或加氢裂化油也可包括在有用的油的范围内。
衍生自煤或页岩的基油可以是有用的。合成润滑油可包括烃油和卤素取代的烃油，例如聚合和共聚烯烃及其混合物、烷基苯、聚苯(例如联苯、三联苯和烷基化聚苯)、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。氧化烯聚合物和共聚体及其衍生物，和其中末端羟基已通过例如酯化或醚化改性的那些可构成可使用的其它类的已知合成润滑油。可使用的其它合适类的合成润滑油包括二羧酸的酯以及由约C5至约C12单羧酸与多元醇或多元醇醚制备的那些。
其它合适合成润滑油可包括含磷酸的液体酯、聚四氢呋喃、硅基油如聚烷基-、聚芳基-、聚烷氧基-或聚芳氧基硅油，和硅酸酯油。
可使用加氢处理的环烷烃油。可使用合成油，例如通过费托反应制备的那些，通常可以为加氢异构化费托烃或蜡。基油可通过费托气至液(gas-to-liquid)合成程序以及其它气至液程序制备。
可使用上文所述类型的天然或合成的未精炼、精炼和再精炼油(及这些中任何两种或更多种的混合物)。未精炼油为不经进一步提纯处理、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。再精炼油可通过将类似于用于得到精炼油的方法应用于已使用的精炼油而得到。通常还将再精炼油通过旨在除去废添加剂和油分解产物的技术加工。
完全配制润滑剂中油的量通常为在计算其余添加剂以后对100%而言余下的量。通常这可以为约60至约99重量%，或约70至约97%，或约80至约95%，或约85至约93重量%。润滑剂组合物可作为浓缩物提供，在这种情况下油的量通常降低且其它组分的浓度相应地提高。在这种情况下，油的量可以为约30至约70重量%，或约40至约60重量%。
VI改进剂
润滑剂组合物含有粘度指数改进量的聚合物，所述聚合物包含衍生自乙烯、丙烯和丁烯的结构单元。该聚合物可通过使包含乙烯、丙烯和丁烯的单体的混合物聚合而制备。这些聚合物可称为共聚物或三聚物。
该聚合物可包含约5至约20摩尔%，或约5至约10摩尔%衍生自乙烯的结构单元；约60至约90摩尔%，或约60至约75摩尔%衍生自丙烯的结构单元；和约5至约30摩尔%，或约15至约30摩尔%衍生自丁烯的结构单元。丁烯可包含其任何异构体或混合物，例如正丁烯、异丁烯或其混合物。丁烯可包含丁烯-1。丁烯的商业来源可包括丁烯-1以及丁烯-2和丁二烯。丁烯可包含丁烯-1和异丁烯的混合物，其中丁烯-1与异丁烯的重量比为约1:0.1或更小。丁烯可包含丁烯-1且不含或基本不含异丁烯。
聚合物可具有约10,000至约500,000；或约30,000至约400,000或约50,000至约350,000，或约150,000至约250,000的数均分子量(如通过凝胶渗透色谱法(GPC)使用聚苯乙烯作为校准标准测定)。聚合物的分子量分布Mw/Mn(如通过GPC使用聚苯乙烯作为校准标准测定，其中Mw为重均分子量，且Mn为数均分子量)可以为约4或更小，或者约3或更小，或者约2.5或更小，或者约2至约4，或约2至约3，或约2至约2.5。
制备聚合物的方法可包括使丙烯、乙烯和丁烯(如丁烯-1)在可进行将烯烃有规立构聚合成全同立构构型或间同立构构型的已知催化剂(例如其主要组分为固体形式的钛组分和有机金属化合物的催化剂或其中金属茂化合物用作催化剂的组分的金属茂催化剂)的存在下聚合。特别地，使用可进行全同立构构型的有规立构聚合的金属茂催化剂的生产方法可用于得到在高温下具有优异燃料效率的润滑剂组合物。这种金属茂催化剂包括国际公开WO2004/106430、国际公开WO2005/019283、国际公开WO2006/025540和国际公开WO2004/087775所述那些。金属茂化合物可包括二苯基亚甲基(3-叔丁基-5-乙基环戊二烯基)(2,7-二-叔丁基芴基)二氯化锆、二苯基亚甲基(3-叔丁基-5-甲基环戊二烯基)(2,7-二-叔丁基芴基)二氯化锆、二甲基亚甲基(3-叔丁基-5-甲基环戊二烯基)(芴基1)二氯化锆等。
聚合物可以以基于重量约0.001至约2%，或约0.003至约1.5%，或约0.005至约1%，或约0.01至约0.75%的浓度存在于润滑剂组合物中。聚合物可以以约0.5至约1%，或约0.6至约0.8重量%的浓度存在。在其它实施方案中，它可以以约0.3至约5重量%或约0.5至约2重量%存在。
聚合物可以以浓缩物提供。浓缩物可包含稀释油和约0.5至约30重量%聚合物，或约1至约15%聚合物，或约5至约15重量%聚合物。
以下实施例显示可用作润滑剂组合物中的粘度指数改进剂的乙烯-丙烯-丁烯聚合物的制备。
实施例1
向装配有搅拌叶片并用氮气彻底洗涤的310L容积加压连续聚合反应器的一个进料开口中以27.1L/hr的流速连续引入提纯且脱水的正己烷。以0.1L/hr的流速连续引入己烷溶液，所述己烷溶液包含37.5毫摩尔/升的浓度的甲基铝氧烷(TMAO-341：TOSOFINECHEMCORPORATION)；0.15毫摩尔/升的浓度的二苯基亚甲基(3-叔丁基-5-乙基环戊二烯基)(2,7-二-叔丁基芴基)二氯化锆；和15.0毫摩尔/升的浓度的三异丁基铝(TiBA：TOSOFINECHEMCORPORATION)。同时向连续聚合反应器的另一进料口中连续加入0.8kg/hr的流速的乙烯、11.1kg/hr的流速的丙烯、6.5kg/hr的流速的丁烯-1和4.5NL/hr(NL=标准升，即在1大气压和0°C下的升)的流速的氢气。连续溶液聚合在其中聚合温度为60°C，总压力为1.0MPa-G(G=表压)且搅拌旋转频率为190rpm的条件下进行。冷却剂通过安装在聚合反应器外部的夹套循环。另外，蒸气相使用分开安装的鼓风机强制循环，蒸气相通过换热器冷却，由此除去聚合热。产生的聚合产物为包含乙烯/丙烯/丁烯-1聚合物的己烷溶液。将该溶液以根据乙烯/丙烯/丁烯-1共聚物7.5kg/hr的速率通过安装在聚合反应器底部的出口取出，使得聚合反应器中溶液的平均量保持在100L。将所得聚合溶液倒入甲醇中以使乙烯/丙烯/丁烯-1聚合物沉淀。将乙烯/丙烯/丁烯-1聚合物在降低的压力下在130°C下干燥24小时。聚合物含有8.7摩尔%衍生自乙烯的结构单元、68摩尔%衍生自丙烯的结构单元和23.3摩尔%衍生自丁烯-1-的结构单元。聚合物具有865kg/m3的密度、47°C的熔点、220,000的Mw，和2.2的Mw/Mn，如通过GPC使用聚苯乙烯作为校准标准测定。
过碱性含金属清净剂
润滑剂组合物可含有一种或多种过碱性含金属清净剂。另外称为过碱性或超碱性盐的过碱性材料可以为单相均匀牛顿体系，其特征是金属含量超过根据金属和与金属反应的具体酸性有机化合物的化学计量将会存在的。过碱性材料可通过酸性材料(通常无机酸或低级羧酸，优选二氧化碳)与包含酸性有机化合物、反应介质、化学计量过量的金属碱和促进剂如氯化钙、乙酸、苯酚或醇的混合物反应而制备，所述反应介质包含至少一种用于所述酸性有机材料的惰性有机溶剂(矿物油、石脑油、甲苯、二甲苯等)。酸性有机材料可具有足够的碳原子数以提供在油中的溶解度。过量金属的量通常根据金属比表示。术语“金属比”为金属的总当量与酸性有机化合物的当量之比。中性金属盐具有1的金属比。具有与正盐中存在的3.5倍一样多的金属的盐具有3.5当量的金属过量，或4.5的比。术语“金属比”还解释于标题为“ChemistryandTechnologyofLubricants”的标准教科书，第2版，R.M.Mortier和S.T.Orszulik编辑，Copyright1997中。
过碱性含金属清净剂的金属可以为锌、钠、钙、钡、镁或其中两种或更多种的混合物。金属可以为钠、钙或镁或其混合物；在一个实施方案中，金属可以为钠和钙的混合物。
过碱性含金属清净剂可选自不含硫的酚盐、含硫酚盐、磺酸盐、salixarate、水杨酸盐及其混合物或其硼酸化等价物。在一个实施方案中，润滑剂组合物可以不含或基本不含苯酚基清净剂。“基本不含”在本文中意指少于10重量%，或少于5或1或0.1重量%的清净剂可以为苯酚基的。可将过碱性清净剂用硼酸化剂如硼酸硼酸化。
过碱性含金属清净剂还可包括用包含酚盐和/或磺酸盐组分的混合表面活性剂体系形成的“混杂”清净剂，例如酚盐-水杨酸盐、磺酸盐-酚盐、磺酸盐-水杨酸盐、磺酸盐-酚盐-水杨酸盐，如例如美国专利6,429,178；6,429,179；6,153,565；和6,281,179所述。如果例如使用混杂磺酸盐-酚盐清净剂，则认为混杂清净剂分别相当于引入相应量酚盐和磺酸盐皂的单独酚盐和磺酸盐清净剂的量。
过碱性含金属清净剂可包括锌、钠、钙或镁的酚盐、含硫酚盐、磺酸盐、salixarate或水杨酸盐。过碱性salixarate、酚盐和水杨酸盐可具有约180至约450TBN的总碱值(ASTMD3896)。过碱性磺酸盐可具有约250至约600，或约300至约500的总碱值。过碱性清净剂是本领域中已知的。磺酸盐清净剂可以为具有至少约8的金属比的主要线性烷基苯或烷基甲苯磺酸盐清净剂，如美国专利公开2005/065045的第[0026]-[0037]段中。线性烷基可以在沿着线性烷基链的任何位置，例如2、3或4位上连接在苯或甲苯上。线性烷基苯磺酸盐清净剂可用于改进燃料经济性。
过碱性含金属清净剂可以为钙或镁过碱性清净剂。润滑剂组合物可包含过碱性磺酸钙、过碱性苯酚钙或其混合物。过碱性清净剂可包含具有至少约3.5，例如约3.5至约40，或约5至约25，或约7至约20的金属比的磺酸钙。
润滑剂组合物可进一步包含低过碱性清净剂(小于约3.5，例如约0至约3.5，或约0.5至约3.0，或约1至约2.5，或约1.5至约2的金属比)或中性清净剂。
过碱性含金属清净剂可以以约0.05至约5重量%的润滑剂组合物的浓度存在于润滑剂组合物中。过碱性清净剂可以以约0.1%、约0.3%，或约0.5%至多约3.2%，或约1.7%，或约0.9重量%的润滑剂组合物的浓度存在。类似地，过碱性清净剂可以以适于提供给润滑剂组合物约1至约10的TBN(总碱值)的量存在。过碱性清净剂可以以提供给润滑剂组合物约1.5至多约3，或至多约5，或至多约7的TBN的量存在。在其它实施方案中，过碱性清净剂可提供给润滑剂组合物至少3的TBN，例如3-7或4-6的TBN。
除TBN外，含金属清净剂也可提供给润滑剂组合物灰。硫酸盐灰(ASTMD874)为常用于表征过碱性清净剂和润滑剂组合物的另一参数。润滑剂组合物可具有约0.3至约1.2重量%，或约0.3至约1.0%或约0.5至约1.0%，或大于约0.6%的硫酸盐灰含量。在其它实施方案中(例如对于船用柴油气缸润滑剂)，灰含量可以为约1至约15%，或约2至约12重量%，或约4至约10%。过碱性清净剂可占约50至约100%的硫酸盐灰，或至少约70%灰，或至少约80%灰，或100%灰。过碱性清净剂可提供不大于约95%的硫酸盐灰，或不大于约98%的硫酸盐灰。
润滑剂组合物可以为船用柴油气缸润滑剂(MDCL)。这类润滑剂的特征可以为主要通过含金属过碱性清净剂提供的高TBN水平。在一些实施方案中，润滑剂组合物可具有至少约10，或至少约20，例如10-100、20-100、30-100、40-80、30-75或40-70的TBN。MDCL组合物的碱度大部分可由清净剂组分贡献，但通常相对少量(例如小于约5%)TBN可由其它物质如含氮分散剂贡献。
其它性能添加剂
润滑剂组合物可包含其它性能添加剂。这些可包括一种或多种金属减活剂、补充粘度改性剂、补充清净剂、摩擦改性剂、抗磨剂、腐蚀抑制剂、分散剂、分散剂粘度改性剂、极压剂、抗氧化剂、抑泡剂、反乳化剂、倾点下降剂、密封溶胀剂、其中两种或更多种的混合物。
抗氧化剂包括硫化烯烃、二芳基胺或烷基化二芳基胺、受阻酚、钼化合物(例如二硫代氨基甲酸钼)、羟基硫醚或其混合物。抗氧化剂可以以约0至约15重量%，或约0.1至约10重量%，或约0.5至约5重量%，或约0.5至约3重量%的润滑剂组合物的浓度存在。
二芳基胺或烷基化二芳基胺可以为苯基-α-萘胺(PANA)、烷基化二苯胺或烷基化苯基萘胺或其混合物。烷基化二苯胺可包括二-壬基化二苯胺、壬基二苯胺、辛基二苯胺、二-辛基化二苯胺、二-癸基化二苯胺、癸基二苯胺及其混合物。在一个实施方案中，二苯胺可包括壬基二苯胺、二壬基二苯胺、辛基二苯胺、二辛基二苯胺或其混合物。在一个实施方案中，二苯胺可包括壬基二苯胺或二壬基二苯胺。烷基化二芳基胺可包括辛基、二-辛基、壬基、二-壬基、癸基或二-癸基苯基萘胺。
受阻酚抗氧化剂可含有仲丁基和/或叔丁基作为位阻基团。苯酚基团可进一步被烃基(通常线性或支化烷基)和/或连接在第二芳族基团上的桥联基团取代。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。受阻酚抗氧化剂可以为酯，例如可以以商品名IrganoxTML-135由Ciba得到的酯。这类材料可由以下通式表示：
其中R3为含有例如1至约18，或2至约12，或2至约8，或2至约6个碳原子的烃基如烷基；且叔烷基可以为叔丁基。可使用的含酯受阻酚抗氧化剂的详细描述可在美国专利6,559,105中找到。
可用作抗氧化剂的二硫代氨基甲酸钼的实例包括以商品名如Vanlube822TM和MolyvanTMA由R.T.VanderbiltCo.,Ltd.,以及AdekaSakura-LubeTMS-100、S-165、S-525和S-600由AsahiDenkaKogyoK.K得到的商业材料及其混合物。
润滑剂组合物可进一步包含一种或多种补充粘度指数改进剂。这些可包括氢化苯乙烯-丁二烯橡胶、乙烯-丙烯共聚物、聚甲基丙烯酸酯、聚丙烯酸酯、氢化苯乙烯-异戊二烯聚合物、氢化二烯聚合物、聚(烷基苯乙烯)、聚烯烃、马来酸酐-烯烃共聚物的酯(例如国际申请WO2010/014655所述那些)、马来酸酐-苯乙烯共聚物的酯，或其中两种或更多种的混合物。
分散剂粘度指数改进剂可包括官能化聚烯烃，例如用酰化剂如马来酸酐和胺官能化的乙烯-丙烯共聚物；用胺官能化的聚甲基丙烯酸酯，或与胺反应的苯乙烯-马来酸酐共聚物。分散剂粘度改性剂的更详细描述公开于国际公开WO2006/015130或美国专利4,863,623；6,107,257；6,107,258；和6,117,825中。分散剂粘度改性剂可包括美国专利4,863,623(参见第2栏第15行至第3栏第52行)或国际公开WO2006/015130(参见第2页，第[0008]段，和制备实施例描述于第[0065]-[0073]段中)所述那些。分散剂粘度改性剂可以以至多约15重量%，或至多约10重量%，或约0.05至约5重量%，或约0.2至约2重量%的润滑剂组合物的浓度存在。
润滑剂组合物可进一步包含一种或多种分散剂。分散剂可以为琥珀酰亚胺分散剂、曼尼希分散剂、琥珀酰胺分散剂、聚烯烃琥珀酸酯、酰胺或酯-酰胺，或其混合物。分散剂可作为单一分散剂存在，或者它可作为两种或更多种(例如三种)不同分散剂的混合物存在，其中至少一种可以为琥珀酰亚胺分散剂。
琥珀酰亚胺分散剂可衍生自一种或多种脂族多胺。脂族多胺可以为脂族多胺如亚乙基多胺(即聚(乙烯胺))、亚丙基多胺、亚丁基多胺或其中两种或更多种的混合物。脂族多胺可以为亚乙基多胺。脂族多胺可选自乙二胺、二亚乙基三胺、三亚乙基四胺、四亚乙基五胺、五亚乙基六胺、多胺釜脚或其中两种或更多种的混合物。
琥珀酰亚胺分散剂可衍生自芳族胺、芳族多胺或其混合物。芳族胺可具有一个或多个通过亚烃基和/或杂原子连接的芳族结构部分，例如4-氨基二苯胺。芳族胺可以为硝基取代的芳族胺。硝基取代芳族胺的实例可包括2-硝基苯胺、3-硝基苯胺和4-硝基苯胺。3-硝基苯胺可以是特别有用的。其它芳族胺可连同硝基苯胺一起存在。与硝基苯胺以及任选与分散橙3(即4-(4-硝基苯基偶氮)苯胺)的缩合产物公开于美国专利公开2006/0025316中。
分散剂可包含用胺官能化的聚合物，例如琥珀酰亚胺分散剂。胺可以为具有至少2，或至少3，或至少4个芳族基团，例如约4至约10，或约4至约8，或约4至约6芳族基团，和至少一个伯或仲氨基，或者，作为另外的选择，至少一个仲氨基的胺。胺可包含伯氨基和至少一个仲氨基。胺可包含至少约4个芳族基团和至少两个仲或叔氨基的任何组合。
具有2个芳族基团的胺的实例为N-苯基-对苯二胺。具有至少3或4个芳族基团的胺的实例可由式(1)表示：
式1
其中各个变量独立地如下：R1可以为氢或C1-5烷基(通常氢)；R2可以为氢或C1-5烷基(通常氢)；U可以为脂族、脂环族或芳族基团(当U为脂族时，脂族基团可以为含有1至约5，或1至约2个碳原子的线性或支化亚烷基)；且w可以为1至约10，或1至约4，或1-2(通常1)。当U为脂族基团时，U可以为含有1至约5个碳原子的亚烷基。作为选择，胺也可由式(1a)表示：
式(1a)
其中各个变量U、R1和R2与上述相同，且w为0至约9，或0至约3，或0至约1(通常0)。
分散剂可以为聚烯烃琥珀酸酯、酰胺或酯-酰胺。例如，聚烯烃琥珀酸酯可以为季戊四醇的聚异丁烯琥珀酸酯或其混合物。聚烯烃琥珀酸酯-酰胺可以为与醇(例如季戊四醇)和胺(例如多胺，通常二亚乙基三胺、多胺釜脚、四亚乙基五胺(TEPA)等)反应的聚异丁烯琥珀酸。
分散剂可以为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为聚异丁烯琥珀酰亚胺，即聚异丁烯取代琥珀酰亚胺分散剂。通常衍生出聚异丁烯琥珀酸酐的聚异丁烯具有约350至约5000，或约550至约3000或约750至约2500的数均分子量。琥珀酰亚胺分散剂和它们的制备例如公开于美国专利3,172,892、3,219,666、3,316,177、3,340,281、3,351,552、3,381,022、3,433,744、3,444,170、3,467,668、3,501,405、3,542,680、3,576,743、3,632,511、4,234,435、Re26,433和6,165,235、7,238,650和EP专利申请0355895A中。
也可将分散剂通过常规方法通过与多种试剂中的任一种反应而后处理。其中，这些为硼化合物(例如硼酸)、脲、硫脲、二巯基噻二唑、二硫化碳、醛、酮、羧酸如对苯二甲酸、烃取代的琥珀酸酐、马来酸酐、腈、环氧化物和磷化合物。可将后处理的分散剂硼酸化。后处理分散剂可由分散剂与二巯基噻二唑反应产生。后处理分散剂可由分散剂与磷酸或亚磷酸反应产生。
分散剂可以以约0.01至约20重量%，或约0.1至约15重量%，或约0.1至约10重量%，或约1至约6重量%，或约1至约3重量%的润滑组合物的浓度存在于润滑剂组合物中。
如果分散剂含有碱性氮原子，则这种碱度可作为分散剂的TBN测量。在一个实施方案中，有用琥珀酰亚胺分散剂的TBN可以基于无油(修正后)为约10至约30，如果基于含有50%油的分散剂试样测量，则其相当于约5至约15。
在一个实施方案中，聚合物的粘度指数改进量(即VI聚合物的量)为约0.5至约2重量%，分散剂的量为约0.01至约20重量%且过碱性磺酸盐的量为约0.05至约5重量%。
摩擦改性剂可选自胺的长链脂肪酸衍生物、长链脂肪酯或长链脂肪环氧化物的衍生物；脂肪咪唑啉；烷基磷酸的胺盐；脂肪烷基酒石酸盐；脂肪烷基酒石酰亚胺；脂肪烷基酒石酰胺；脂肪甘醇酸酯；和脂肪2-羟乙酰胺。如本文所用，与摩擦改性剂有关的术语“脂肪烷基或脂肪”意指具有约10至约22个碳原子的碳链，通常直碳链。作为选择，可使用单支化烷基替代脂肪烷基。典型的单支化烷基可包括β-支化基团如2-乙基己基、2-丙基庚基等。摩擦改性剂可以以0至约6重量%，或约0.01至约4重量%，或约0.05至约2重量%，或约0.1至约2重量%的润滑剂组合物的浓度存在于润滑剂组合物中。
可使用的摩擦改性剂的实例可包括脂肪酯、脂肪环氧化物或胺的长链脂肪酸衍生物；脂肪咪唑啉如羧酸和聚亚烷基多胺的缩合产物；烷基磷酸的胺盐；脂肪烷基酒石酸盐；脂肪烷基酒石酰亚胺；脂肪烷基酒石酰胺；脂肪膦酸盐；脂肪亚磷酸盐；硼酸化磷脂、硼酸化脂肪环氧化物；甘油酯；硼酸化甘油酯；脂肪胺；烷氧基化脂肪胺；硼酸化烷氧基化脂肪胺；羟基和聚羟基脂肪胺，包括叔羟烷基脂肪胺；羟基烷基酰胺；脂肪酸的金属盐；烷基水杨酸盐的金属盐；脂肪噁唑啉；脂肪乙氧基化醇；羧酸和聚亚烷基多胺的缩合产物；或脂肪羧酸与胍、氨基胍、脲或硫脲及其盐的反应产物。
摩擦改性剂还可包括材料如硫化脂肪化合物和烯烃、二烷基二硫代磷酸钼、二硫代氨基甲酸钼、多元醇和衍生自或可衍生自向日葵油或豆油的脂肪羧酸的单酯。
摩擦改性剂可以为长链脂肪酸酯。长链脂肪酸酯可以为单酯、二酯、(三)甘油酯或其中两种或更多种的混合物。
润滑剂组合物可任选进一步包含至少一种抗磨剂。合适抗磨剂的实例可包括酒石酸盐、酒石酰亚胺、磷化合物的油溶性胺盐、硫化烯烃、金属二烃基二硫代磷酸盐(例如二烷基二硫代磷酸锌)、亚磷酸盐(例如二丁基亚磷酸盐)、膦酸盐、含硫代氨基甲酸酯的化合物，例如硫代氨基甲酸酯、硫代氨基甲酸酰胺、硫代氨基甲酸醚、亚烷基偶联的硫代氨基甲酸酯和双(S-烷基二硫代氨基甲酰基)二硫醚。在一个实施方案中，抗磨剂可包括如国际公开WO2006/044411或加拿大专利CA1183125所公开的酒石酸盐或酒石酰亚胺。酒石酸盐或酒石酰亚胺可含有烷基，其中烷基上的碳原子之和为至少约8。
另一类添加剂可包括如美国专利7,727,943和美国专利公开2006/0014651所公开的油溶性钛化合物。这些可充当抗磨剂、摩擦改性剂、抗氧化剂、沉积物控制添加剂等。这些添加剂可以为多功能添加剂。例如这些添加剂中的一种可提供抗磨和抗氧化剂性能。油溶性钛化合物可以为钛(IV)醇盐。钛醇盐可由一元醇、多元醇或其混合物形成。一元醇盐可具有2至约16个碳原子，或3至约10个碳原子。钛醇盐可以为异丙醇钛(IV)。钛醇盐可以为2-乙基己醇钛(IV)。钛化合物可包括连1,2-二醇或多元醇的醇盐。1,2-连二醇可包括甘油的脂肪酸单酯，例如油酸酯。
油溶性钛化合物可以为钛羧酸盐。钛羧酸盐可衍生自钛醇盐和羧酸，所述羧酸选自非线性单羧酸和具有多于约22至多约25个碳原子的羧酸。钛/羧酸产物的实例可包括与酸的钛反应产物，所述酸选自己酸、辛酸、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、花生酸、油酸、芥酸、亚油酸、亚麻酸、环己烷羧酸、苯乙酸、苯甲酸、新癸酸等。制备这类钛/羧酸产物的方法例如描述于美国专利5,260,466中。
可溶于油中的极压(EP)剂可包括含硫和含氯硫的EP剂、分散剂(通常琥珀酰亚胺分散剂)的二巯基噻二唑或CS2衍生物、氯化烃EP剂和磷EP剂的衍生物。这类EP试剂的实例可包括氯化蜡；硫化烯烃(例如硫化异丁烯)、烃基取代的2,5-二巯基-1,3,4-噻二唑或其低聚物、有机硫化物和聚硫化物如二苄基二硫醚、双-(氯苄基)二硫醚、二丁基四硫、油酸的硫化甲酯、硫化烷基苯酚、硫化二戊烯、硫化萜烯和硫化Diels-Alder加合物；磷硫化烃如硫化磷与松节油或油酸甲酯的反应产物；磷酯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、亚磷酸戊基苯基酯；亚磷酸二戊基苯基酯、亚磷酸十三烷基酯、二硬脂醇亚磷酸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；烷基和二烷基磷酸或衍生物的胺盐，包括例如二烷基二硫代磷酸与氧化丙烯反应，其后进一步与P2O5反应的反应产物的胺盐；及其混合物(如US3,197,405所述)。
可用于润滑剂组合物中的抑泡剂可包括聚硅氧烷，丙烯酸乙酯、丙烯酸2-乙基己酯以及任选乙酸乙烯酯的共聚物；反乳化剂，包括氟化聚硅氧烷、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。
可用于润滑剂组合物中的倾点下降剂可包括聚α烯烃、马来酸酐-苯乙烯共聚物的酯、聚(甲基)丙烯酸酯、聚丙烯酸酯或聚丙烯酰胺。
可使用反乳化剂可包括磷酸三烷基酯，和乙二醇、氧化乙烯、氧化丙烯或其中两种或更多种的混合物的各种聚合物和共聚物。
金属减活剂可包括苯并三唑的衍生物(通常甲苯基三唑)、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。金属减活剂也可描述为腐蚀抑制剂。
可使用的密封溶胀剂可包括sulfolene衍生物如ExxonNecton-37TM(FN1380)和ExxonMineralSealOilTM(FN3200)。
工业应用
润滑剂组合物可用于通过将如本文所述润滑剂供入装置中而润滑机械装置。装置可以为内燃机如汽油燃烧或柴油燃烧汽车发动机，重型柴油机、船用柴油机或固定式燃气发动机。这类发动机可以为油底壳润滑的，且润滑剂可从它可以润滑发动机的移动部件处供入油底壳中。或者，润滑剂可由不是油底壳的一部分的分开来源供入。
内燃机可以为柴油燃烧发动机(通常重型柴油机)、汽油燃烧发动机、天然气燃烧发动机、混合汽油/醇燃烧发动机或氢气燃烧内燃机。内燃机可以为柴油燃烧发动机或汽油燃烧发动机。内燃机可以为重型柴油机。
内燃机可以为2冲程或4冲程发动机。合适的内燃机可包括船用柴油机(其可包含用所述润滑剂润滑的气缸)、航空用活塞式发动机、低载荷柴油机和汽车和卡车发动机。船用柴油机可以用船用柴油气缸润滑剂(通常在2冲程发动机中)、系统油(通常在2冲程发动机中)或曲轴箱润滑剂(通常在4冲程发动机中)润滑。
一类内燃机为直接注入式燃机，其中将燃料直接注入气缸中。直接注入的具体实例可包括壁引导和喷雾引导直接注入式发动机。可使用润滑剂组合物润滑汽油直接注入式发动机。
润滑剂组合物可适用作任何发动机润滑剂，而不管硫、磷或硫酸盐灰含量。当用作发动机油时，润滑剂组合物的硫含量可以为约1重量%或更少，或者约0.8重量%或更少，或者约0.5重量%或更少，或者约0.3重量%或更少。硫含量可以为约0.001至约0.5重量%，或约0.01至约0.3重量%。磷含量可以为约0.2重量%或更少，或者约0.12重量%或更少，或者约0.1重量%或更少，或者约0.085重量%或更少，或者约0.08重量%或更少，或者约0.06重量%或更少，或者约0.055重量%或更少，或者约0.05重量%或更少。磷含量可以为约0.04至约0.12重量%。磷含量可以为约100ppm至约1000ppm，或约200ppm至约600ppm。总硫酸盐灰含量可以为约0.3重量-1.2重量%，或约0.5至约1.1重量%的润滑剂组合物。硫酸盐灰含量可以为约0.5重量-1.1重量%的润滑剂组合物。润滑剂组合物的特征可以为至多约100ppm，或至多约50ppm，或至多约10ppm的氯含量。
润滑剂组合物可以为发动机油，其中润滑剂组合物的特征可以为具有如下至少一项：(i)润滑剂组合物的约0.5重量%或更少的硫含量，(ii)约0.12重量%或更少的磷含量，和(iii)约0.5至约1.1重量%的硫酸盐灰含量。
润滑剂组合物可以为船用柴油气缸润滑剂，其可用于润滑船用柴油气缸。船用柴油气缸可以在二冲程船用柴油机中。船用柴油气缸润滑剂通常用于一次通过并被消耗，而不是保留在油底壳中。这些润滑剂可能需要高清净剂含量，赋予润滑剂高碱度水平，如通过TBN测量，通常产生约20或更大，例如约30或更大，或者约40或更大，或者约50或更大，或者约70或更大，且通常至多约80，或至多约100，或至多约300的TBN水平。
润滑剂组合物可用于操作内燃机的方法中，其中活塞沉积物评价提高且粘度的增加降低。
在一个实施方案中，所公开的技术提供降低内燃机中的活塞沉积物水平的方法，所述方法包括用如本文所述润滑剂组合物润滑发动机。在一个实施方案中，所公开的技术提供
粘度指数改进量的聚合物在润滑剂组合物中的用途，所述聚合物包含约5至约20摩尔%衍生自乙烯的结构单元、约50至约90摩尔%衍生自丙烯的结构单元和约5至约30摩尔%衍生自丁烯的结构单元，所述润滑剂组合物进一步包含具有润滑粘度的油、分散剂；和包含过碱性磺酸盐的清净剂，其中磺酸盐具有约250至约600的总碱值，以降低通过所述润滑剂组合物润滑的发动机中的活塞沉积物水平。
实施例2
将完全配制发动机油与根据实施例1中的公开内容制备的聚合物(下文中聚合物1)和市售烯烃共聚物(下文中对比OCP或CompOCP)混合，并测试“非粘度测试”优点。在ASTMSequenceIIIG试验中，当使用聚合物1时，存在与CompOCP相比显著的沉积物性能改进。聚合物1和CompOCP具有表1所示性能。
表1–聚合物组成
| 聚合物1 | Comp OCP | |
| 乙烯(摩尔%) | 8.7 | 57 |
| 丙烯(摩尔%) | 68.0 | 43 |
| 丁烯(摩尔%) | 23.3 | 0 |
| Mw | 220,000 | 290,000 |
| 剪切稳定性指数 | 35 | 45 |
使用表1的聚合物制备表2所示发动机油(EO)配制剂。使用聚合物1配制EONo.1。使用CompOCP配制CompEO。在表2中，向混合油提供一些添加剂，并显示这些的混合油重量百分数。另外，在表2中，除非另外指出，所有数值以重量份表示(所有百分数为重量计)。
表2–发动机油(EO)配制剂
使用表2所示发动机油配制剂进行ASTMSequenceIIIG试验。这些试验结果显示于表3中。
表3–ASTMSequenceIIIG试验结果
| EO No.1 | Comp EP | |
| 粘度等级 | 5W-30 | 5W-30 |
| 100°C下的基油粘度(cSt) | 4.8 | 4.9 |
| 润滑剂组合物在100°C下的运动粘度(cSt) | 9.83 | 10.3 |
| 高温、高剪切粘度(cP)ASTMD4683 | 2.87 | 3.02 |
| 冷起动模拟机(cP，在-30°C下)ASTM D4684 | 6324 | 6152 |
| 粘度提高 | 76.9% | 138% |
| 称重活塞沉积物评定 | 4.05 | 3.88 |
这些试验结果显示当使用EONo.1时，与CompEO相比显著提高的活塞沉积物评定和发动机油中显著的稠化降低。
尽管已关于各个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，应当理解本发明包括可属于所附权利要求书范围的所有这类改进。
除非另外指出，例如除非指明油的量，所述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(即基于活性化学品)。然而，除非另外指出，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。
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。例如，金属离子(例如清净剂的)可迁移至其它分子的其它酸性或阴离子部位。由此形成的产品，包括经以其意欲用途使用本发明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组合物。
将以上提及的各文件通过引用并入本发明，包括要求保护优先权的任何现有申请，无论上文中是否具体列出。任何文件的提及不是承认该文件取得现有技术的资格或以任何权限构成技术人员的常识。除实施例中，或另外明确指出外，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。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。如本文所用，表述“基本由…组成”允许包括不本质上影响所考虑组合物的基本特征和新特征的物质。
Claims (15)
1.润滑剂组合物，其包含：
至少60重量％的具有润滑粘度的油；
0.001至2重量％的粘度指数改进量的聚合物，所述聚合物包含5至20摩尔％衍生自乙烯的结构单元、50至90摩尔％衍生自丙烯的结构单元和5至30摩尔％衍生自丁烯的结构单元；
0.01至20重量％的琥珀酰亚胺分散剂；和
0.05至5重量％清净剂，其包含过碱性钙、镁或钠磺酸盐，其中磺酸盐具有250至600的总碱值。
2.根据权利要求1的组合物，其中聚合物的粘度指数改进量为0.5至2重量％。
3.根据权利要求1的组合物，其中分散剂包含聚异丁烯取代琥珀酰亚胺分散剂。
4.根据权利要求1的组合物，其中过碱性磺酸盐以适于提供给润滑剂组合物1至10的TBN(总碱值)的量存在。
5.根据权利要求1的组合物，其中组合物进一步包含抗磨剂、抗氧化剂、摩擦改性剂、倾点下降剂和消泡剂中的至少一种。
6.根据权利要求1的组合物，其中组合物进一步包含一种或多种金属减活剂、其它补充粘度改性剂、补充清净剂、腐蚀抑制剂、分散剂粘度改性剂、极压剂、反乳化剂、密封溶胀剂，或者其中两种或更多种的混合物。
7.根据权利要求1的组合物，其中具有润滑粘度的油包含组II油。
8.根据权利要求1的组合物，其中具有润滑粘度的油具有在100℃下小于5cSt的运动粘度和小于130的粘度指数。
9.根据权利要求1的组合物，其中聚合物具有10,000至500,000的数均分子量。
10.根据权利要求1的组合物，其中聚合物具有4或更小的Mw/Mn。
11.根据权利要求1的组合物，其中聚合物包含5至10摩尔％衍生自乙烯的结构单元、60至75摩尔％衍生自丙烯的结构单元、15至30摩尔％衍生自丁烯的结构单元、150,000至250,000的数均分子量和2至2.5的Mw/Mn。
12.根据权利要求1的组合物，其中组合物具有1重量％或更少的硫含量、0.2重量％或更少的磷含量和0.3至1.2重量％的硫酸盐灰含量。
13.润滑内燃机的方法，其包括：向发动机中供入根据前述权利要求中任一项的润滑剂组合物。
14.降低内燃机中的活塞沉积物水平的方法，其包括用根据权利要求1至12中任一项的润滑剂组合物润滑发动机。
15.0.001至2重量％的粘度指数改进量的聚合物的用途，用于润滑剂组合物中，用于降低通过所述润滑剂组合物润滑的发动机中的活塞沉积物水平，所述聚合物包含5至20摩尔％衍生自乙烯的结构单元、50至90摩尔％衍生自丙烯的结构单元和5至30摩尔％衍生自丁烯的结构单元，所述润滑剂组合物进一步包含至少60重量％的具有润滑粘度的油、0.01至20重量％的琥珀酰亚胺分散剂；和0.05至5重量％的清净剂，所述清净剂包含过碱性钙、镁或钠磺酸盐，其中磺酸盐具有250至600的总碱值。
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| CN108641790A (zh) * | 2018-04-28 | 2018-10-12 | 山东源根化学技术研发有限公司 | 一种燃气发动机润滑油组合物及其制备方法 |
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| EP2649167B1 (en) | 2016-03-09 |
| BR112013014297A2 (pt) | 2016-09-20 |
| JP5897030B2 (ja) | 2016-03-30 |
| CN103354832A (zh) | 2013-10-16 |
| WO2012078572A1 (en) | 2012-06-14 |
| SG190994A1 (en) | 2013-07-31 |
| KR20130130003A (ko) | 2013-11-29 |
| JP2013544948A (ja) | 2013-12-19 |
| KR101815338B1 (ko) | 2018-01-30 |
| CA2820583A1 (en) | 2012-06-14 |
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