CN103180419B - 含芳族分散剂和钛的润滑剂 - Google Patents
含芳族分散剂和钛的润滑剂 Download PDFInfo
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- CN103180419B CN103180419B CN201180050832.9A CN201180050832A CN103180419B CN 103180419 B CN103180419 B CN 103180419B CN 201180050832 A CN201180050832 A CN 201180050832A CN 103180419 B CN103180419 B CN 103180419B
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- aromatic
- lubricant
- oil
- titanium
- lubricant compositions
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- 239000000314 lubricant Substances 0.000 title claims abstract description 67
- 125000003118 aryl group Chemical group 0.000 title claims abstract description 56
- 239000002270 dispersing agent Substances 0.000 title claims abstract description 30
- 239000010936 titanium Substances 0.000 title claims description 35
- 229910052719 titanium Inorganic materials 0.000 title claims description 27
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 26
- 239000000203 mixture Substances 0.000 claims abstract description 61
- 229920000642 polymer Polymers 0.000 claims abstract description 47
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 24
- 239000007859 condensation product Substances 0.000 claims abstract description 20
- 150000001408 amides Chemical class 0.000 claims abstract description 14
- 150000003949 imides Chemical class 0.000 claims abstract description 11
- 230000001050 lubricating effect Effects 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 73
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- 239000006185 dispersion Substances 0.000 claims description 35
- 229920002367 Polyisobutene Polymers 0.000 claims description 29
- 150000004982 aromatic amines Chemical class 0.000 claims description 25
- 229910052751 metal Inorganic materials 0.000 claims description 24
- 239000002184 metal Substances 0.000 claims description 24
- 238000000746 purification Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- RINCXYDBBGOEEQ-UHFFFAOYSA-N succinic anhydride Chemical group O=C1CCC(=O)O1 RINCXYDBBGOEEQ-UHFFFAOYSA-N 0.000 claims description 15
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- 238000000034 method Methods 0.000 claims description 13
- 239000000654 additive Substances 0.000 claims description 12
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- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 claims description 8
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- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
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- DKVNPHBNOWQYFE-UHFFFAOYSA-N carbamodithioic acid Chemical compound NC(S)=S DKVNPHBNOWQYFE-UHFFFAOYSA-N 0.000 claims 1
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- 239000002199 base oil Substances 0.000 description 7
- 239000010705 motor oil Substances 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 229920000768 polyamine Polymers 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
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- ATGUVEKSASEFFO-UHFFFAOYSA-N p-aminodiphenylamine Chemical compound C1=CC(N)=CC=C1NC1=CC=CC=C1 ATGUVEKSASEFFO-UHFFFAOYSA-N 0.000 description 5
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- 125000001302 tertiary amino group Chemical group 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 230000002378 acidificating effect Effects 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 239000003599 detergent Substances 0.000 description 4
- 229940035422 diphenylamine Drugs 0.000 description 4
- VYFOAVADNIHPTR-UHFFFAOYSA-N isatoic anhydride Chemical compound NC1=CC=CC=C1CO VYFOAVADNIHPTR-UHFFFAOYSA-N 0.000 description 4
- 239000002480 mineral oil Substances 0.000 description 4
- 235000010446 mineral oil Nutrition 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
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- CQRYARSYNCAZFO-UHFFFAOYSA-N salicyl alcohol Chemical compound OCC1=CC=CC=C1O CQRYARSYNCAZFO-UHFFFAOYSA-N 0.000 description 4
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- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 4
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- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 description 1
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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
- C10M149/00—Lubricating compositions characterised by the additive being a macromolecular compound containing nitrogen
- C10M149/12—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C10M149/14—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds a condensation reaction being involved
- C10M149/22—Polyamines
-
- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/02—Well-defined hydrocarbons
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/10—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms
- C10M105/12—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to acyclic or cycloaliphatic carbon atoms monohydroxy
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/16—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen having hydroxy groups bound to a carbon atom of a six-membered aromatic ring
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/20—Aldehydes; Ketones
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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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/22—Carboxylic acids or their salts
- C10M105/24—Carboxylic acids or their salts having only one carboxyl group bound to an acyclic carbon atom, cycloaliphatic carbon atom or hydrogen
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/22—Carboxylic acids or their salts
- C10M105/26—Carboxylic acids or their salts having more than one carboxyl group bound to an acyclic carbon atom or cycloaliphatic carbon atom
-
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/22—Carboxylic acids or their salts
- C10M105/28—Carboxylic acids or their salts having only one carboxyl group bound to a carbon atom of a six-membered aromatic ring
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- 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
- C10M105/00—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound
- C10M105/08—Lubricating compositions characterised by the base-material being a non-macromolecular organic compound containing oxygen
- C10M105/32—Esters
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
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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
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
- C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
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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
- C10M129/00—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen
- C10M129/02—Lubricating compositions characterised by the additive being an organic non-macromolecular compound containing oxygen having a carbon chain of less than 30 atoms
- C10M129/26—Carboxylic acids; Salts thereof
- C10M129/28—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms
- C10M129/38—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms
- C10M129/40—Carboxylic acids; Salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having 8 or more carbon atoms monocarboxylic
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Abstract
一种润滑剂组合物，其包含具有润滑粘度的油；包含羧基官能化聚合物经由酰胺、酰亚胺、或酯键与芳族结构部分的缩合产物；和油溶性钛化合物，呈现良好氧化稳定性。
Description
背景技术
本公开技术涉及具有良好氧化稳定性的润滑剂，其包含油溶性钛化合物和羧基官能化聚合物与芳族结构部分的缩合产物的组合。
发动机制造厂为了将颗粒排放、其他污染物的排放减到最少，并且同时改进清洁度、燃料经济性、和效率，已经关注改进发动机设计。发动机设计中的一个改进为使用废气再循环(EGR)发动机。发动机设计和操作的改进有助于减少排放的同时，某些发动机设计改进被认为已经对润滑剂产生其它挑战。例如，EGR被认为已经导致煤烟和淤泥的增加的形成和/或累积。
煤烟作为媒介的油增稠在重型柴油发动机中常见。某些柴油发动机采用EGR。EGR发动机中形成的煤烟具有不同结构并且在比无EGR的发动机中形成的煤烟更低浓度下，引起发动机润滑剂的增加粘度。减轻煤烟作为媒介的油增稠的尝试已包括使用包含芳族官能团的分散剂，例如公开在2010年6月3日的PCT公开WO2010/062842；2006年2月2日，Covitch等人的美国申请2006-0025316；或2006年8月24日Bera等人的美国申请2006-0189492中。
同时，已经存在提供满足政府技术规范、例如降低的硫和磷限制的曲轴箱润滑剂的持续兴趣。普遍认为，降低这些限制可能对发动机性能、发动机磨损和发动机用油的氧化造成严重影响。这是因为过去发动机油中磷含量的主要来源为二烷基二硫代磷酸锌(ZDP)，并且长期以来ZDP被用于赋予发动机油耐磨和氧化稳定性能。因此，由于期望降低发动机油中的ZDP量，需要替代品以防止发动机性能、发动机磨损和发动机油氧化的一种或多种性能变差。无论润滑剂中是否包含ZDP和相关材料，这种改进的保护是令人期望的。解决这些问题的润滑剂已经配制包含油溶性钛化合物，如公开在2010年6月1日Rrown等人的美国专利7,727,943、和2009年11月10日Esche,JR的7,615,520中。
然而，仍然需要具有例如如上所述的良好或改进性能，包括进一步改进的氧化稳定性的润滑剂。本文公开的技术提供具有一种或多种此类性能的润滑剂。
发明概述
本公开技术提供润滑剂组合物，其包含(a)具有润滑粘度的油；(b)与包含羧基官能化聚合物经由酰胺、酰亚胺、或酯键与芳族结构部分的缩合产物；和(c)油溶性钛化合物。
本公开技术进一步提供润滑机械装置的方法，包括将上述润滑剂组合物供入所述装置。
本公开技术进一步提供改进用于机械装置的润滑剂氧化稳定性的方法，包括在所述润滑剂中包含(b)具有羧基官能化聚合物经由酰胺、酰亚胺或酯键与芳族结构部分的缩合产物的分散剂；和(c)油溶性钛化合物。
发明详述
下面通过非限制性说明描述各种优选的特征和实施方案。
除非另有说明，所述的各化学组分的量不包括可能通常在该商业材料中存在的任何溶剂或稀释剂油，即基于活性化学物质。然而，除非另有说明，本文提到的各化学品或组合物应理解为商品级材料，其可包含异构体、副产物、衍生物、和通常理解为存在于该商品级中的其它此类材料。
本文中所用的术语“烃基取代基”或“烃基”以本领域技术人员熟知的一般含义使用。特别地，其指具有直接连接分子其余部分的碳原子并主要具有烃性质的基团。烃基的实例包括：烃取代基，包括脂族、脂环族、和芳族取代基；取代的烃取代基，即包含在本发明的范围内不会改变取代基的主要烃特征的非烃基基团的取代基；以及杂取代基，即类似地主要具有烃性质但是在环或链中包含非碳的取代基。术语“烃基取代基”或“烃基”的更详细定义发现在国际公开WO2008147704的-段中。
本公开技术的一种组分为具有润滑粘度的油。用于本发明的润滑油组合物中的基础油可选自如在美国石油学会(API)基础油互换性指南中规定的I-V类中的任何基础油。这5种基础油类别如下：
在一个实施方案中，本技术中使用的基础油具有少于300ppm硫和/或至少90%饱和物含量，通过ASTM D2007测得。在某些实施方案中，基础油具有至少95或至少115的粘度指数。
I、II和III类为矿物油基础油料。因而，具有润滑粘度的油可包括天然或合成润滑油及其混合物。常使用矿物油和合成油的混合物，特别是聚α烯烃油和聚酯油。
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，例如液体石油和溶剂处理过的或酸处理过的链烷、环烷、或者混合链烷-环烷型矿物润滑油。加氢处理或加氢裂化的油包括在可用的具有润滑粘度的油的范围内。
衍生自煤炭或页岩的具有润滑粘度的油也可用。合成润滑油包括烃油和卤代烃油，例如聚合和共聚的烯烃及其混合物、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醚和它们的衍生物、类似物和同系物。氧化烯聚合物和共聚物及其衍生物、以及其中末端羟基已通过例如酯化或醚化改性的那些，构成可用的已知合成润滑油的其它种类。可用的另一种合适的合成润滑油包括二羧酸的酯、和由C5-C12一元羧酸与多元醇或多元醇醚制成的那些。
其它合成润滑油包括含磷的酸的液体酯、聚合四氢呋喃、硅基油，如聚烷基-、聚芳基-、聚烷氧基、或聚芳氧基-硅氧烷油、和硅酸酯油。
加氢处理的环烷油也是已知并且可用的。可使用合成油，例如通过Fischer-Tropsch反应生产的那些，并且通常可为加氢异构的Fischer-Tropsch烃或蜡。在一个实施方案中，油可通过Fischer-Tropsch气-液合成方法制备以及其他气-液油。
上文公开类型的未精制、精制和再精制的油，天然的或合成的(以及这些中任何两种或更多种的混合物)，可用于本发明的组合物中。未精制的油为直接从天然或合成来源得到而未进一步提纯处理的那些。精制油类似未精制油，不同之处在于前者已经在一个或多个提纯步骤中进一步处理以改进一种或多种性能。再精制油通过对已经使用过的精制油施用与获得精制油类似的那些方法获得。这种再精制油通常另外通过用于除去废添加剂和油分解产物的技术加工。
计算剩余添加剂后，在完全配制的润滑剂中的油的量通常为至100%的剩余量。通常它可为60-99重量%、或70-97%、或80-95%、或85-93%。本公开的技术还可作为浓缩物提供，在这样情况下油的量通常降低，而其他组分的浓度相应增加。在这种情况下，油的量可为30-70重量%或40-60%。
聚合分散剂
本发明的润滑组合物包含分散剂，其含有羧基官能化聚合物经由酰胺、酰亚胺、或酯键与芳族结构部分的缩合产物。即，其可为与任何各种类型的芳族胺的缩合产物。如果通过芳族胺的氮原子缩合，可形成酰胺或酰亚胺键。或者，分散剂可为与任何各种类型的芳香醇或酚的缩合产物(包括可看作醇或酚的反应等同物的酯)。如果通过芳香醇或酚的氧原子缩合，可形成酯键。如果芳族化合物包含胺和醇官能团两者，那么可形成任何酰胺、酰亚胺、或酯，或其混合物，取决于反应条件和是否主要在胺或醇基进行反应。
在某些实施方案中，分散剂包含用某种胺官能化的聚合物。用于聚合分散剂的胺通常为具有至少2个或至少3个或至少4个芳基基团的胺，例如4-10、或4-8、或4-6个芳基基团，和至少一个伯或仲氨基，或者至少一个仲氨基。在某些实施方案中，胺包含伯和至少一个仲氨基二者。在某些实施方案中，胺包含至少4个芳基基团和至少2个仲或叔氨基(即仲和/或叔氨基总计至少2个的任何组合)。
本文中所用的术语“芳基”以一般术语含义使用并且已知由每一环体系4n+2π电子的Hückel理论所定义。因此，本发明的一个芳基可具有6、或10、或14个π电子。苯环具有6个π电子，萘环具有10个π电子，和吖啶基具有14个π电子。
具有2个芳基基团的胺的实例为N-苯基-对苯二胺(又称为4-氨基二苯基胺，ADPA)。具有至少3或4个芳基基团的胺的实例可由式(1)表示：
其中，独立地，各个变量如下：R1可为氢或C1-5烷基(通常为氢)；R2可为氢或C1-5烷基(通常为氢)；U可为脂基、脂环基或芳基(当U为脂基时，该脂基可为包含1-5、或1-2个碳原子的线性或支化的亚烷基)；且w可为1-10、或1-4、或1-2(通常为1)。在一个实施方案中，当U为脂族基时，U尤其为包含1-5个碳原子的亚烷基。
或者，具有至少3或4个芳基基团的胺的实例可通过式(1a)所示的结构表示：
其中各个变量U、R1、和R2如上所述并且在这一表达式中w为0-9或0-3或0-1(典型地为0)。
具有至少3或4个芳基基团的胺的进一步实例可由以下式(2)和/或(3)的任一表示：
相对亚烷基桥键具有各种氨基位置的异构体也可用，仅作为一个实例，包括式(2x)的那些：
在一个实施方案中，具有至少3或4个芳基基团的胺可包括由以上公开的式表示的化合物的混合物。本领域技术人员知道式(2)和(3)的化合物还可与下述的醛反应形成吖啶衍生物，包括由式以下式(2a)或(3a)-(3c)表示的那些。除了这些式表示的化合物以外，当醛与其它以>NH基桥接的苄基反应时，其它吖啶结构可用。
任一或所有的N-桥接芳族环能够这样进一步缩合并且或许芳构化。许多可用的结构的另一种显示在式(3b)中。
任一式(2)、(2a)、(3)、或(3a)-(3c)也可进一步产生缩合反应，导致每一分子形成一个或多个吖啶结构部分。
具有至少3或4个芳基基团的胺的实例包括双[对-(对-氨基苯胺)苯基]-甲烷、2-(7-氨基-吖啶-2-基甲基)-N-4-{4-[4-(4-氨基-苯基氨基)-苄基]-苯基}苯-1,4-二胺、N-4-{4-[4-(4-氨基-苯基氨基)-苄基]-苯基}-2-[4-(4-氨基-苯基氨基)-环己-1,5-二烯基甲基]-苯-1,4-二胺、N-[4-(7-氨基-吖啶-2-基甲基)-苯基]-苯-1,4-二胺、及其混合物。在一个实施方案中，具有至少3或4个芳基基团的胺可为双[对-(对-氨基-苯胺基)苯基]-甲烷、2-(7-氨基-吖啶-2-基甲基)-N-4-{4-[4-(4-氨基-苯基氨基)-苄基]-苯基}-苯-1,4-二胺或其混合物。
具有至少2或3或4个芳基基团的胺可通过包括使醛与胺(典型地4-氨基二苯基胺)反应的方法制备。所得的胺可描述为具有至少2或3或4个芳基基团的亚烷基偶联的胺，在某些实施方案中，至少一个-NH2官能团和至少2个仲或叔氨基。用于偶联的醛可为脂族、脂环族、或芳族。脂族醛可为直链或支化的。合适的芳族醛的实例包括苯甲醛和o-香草醛。脂族醛的实例包括甲醛(或其反应性的同等物，例如***或多聚甲醛)、乙醛、和丙醛。典型地，醛可为甲醛或苯甲醛。另外，具有至少3或4个芳基基团的胺还可通过Berichte der Deutschen Chemischen Gesellschaft(1910),43,728-39中记载的方法制备。
在一个实施方案中，具有至少3或4个芳基基团的胺可通过或通过以下方法获得，即包括使靛红酸酐或烷基取代的靛红酸酐与具有至少两个芳基基团和反应性伯或仲氨基的芳族胺反应。所得的材料可描述为邻氨基苯甲酸衍生物。
在一个实施方案中，邻氨基苯甲酸衍生物可通过使靛红酸酐或烷基取代的靛红酸酐和选自二甲苯二胺、4-氨基二苯基胺、1,4-二甲基亚苯基二胺、及其混合物反应制备。在一个实施方案中，芳族胺可为4-氨基二苯基胺。
如上所述制备邻氨基苯甲酸衍生物的方法可在20°C-180°C、或40°C-110°C的反应温度下进行。该方法可以(或可以不)在溶剂的存在下进行。合适的溶剂的实例包括水、稀释油、苯、叔丁基苯、甲苯、二甲苯、氯苯、己烷、四氢呋喃、或其混合物。反应可在空气或惰性气氛例如氮气或氩气，典型地氮气中进行。
在其它实施方案中，芳族胺可为硝基取代的芳族胺。硝基取代的芳族胺的实例包括2-硝基苯胺、3-硝基苯胺、和4-硝基苯胺。3-硝基苯胺尤其可用。其他芳族胺可与硝基苯胺一起提供。与硝基苯胺且任选还与DisperseOrange3(即4-(4-硝基苯基偶氮)苯胺)的缩合产物自2006年2月2日公开的Covitch等人的美国专利申请2006-0025316已知。
羧基官能化聚合物
本技术的分散剂可为如上所述的芳族胺或醇与羧基官能化聚合物的反应产物。所得产物可描述为胺官能化的羧基官能化聚合物。羧基官能化聚合物可包括含一个或多个羧基(或等效物)的烯烃聚合物。羧基官能化聚合物主链可为均聚物或共聚物，前提是它包含至少一个羧酸官能团或羧酸官能团的反应性等同物(例如酐或酯)。羧基官能化聚合物可具有在主链上接枝、在聚合物主链内部或作为聚合物主链上的端基的羧酸官能团(或羧酸官能团的反应性等同物)。
羧基官能化聚合物可为聚异丁烯取代的琥珀酸酐、马来酸酐-苯乙烯共聚物、马来酸酐-苯乙烯共聚物的酯、α-烯烃-马来酸酐共聚物、或(i)苯乙烯-乙烯-α烯烃聚合物、(ii)氢化的烯基芳基共轭二烯共聚物(即氢化的烯基芳烃共轭二烯共聚物，尤其是苯乙烯-丁二烯的氢化共聚物)、(iii)接枝马来酸酐的聚烯烃(尤其是乙烯-丙烯共聚物)、或(iv)异戊二烯聚合物(尤其是未氢化的异丁烯或氢化苯乙烯-异戊二烯聚合物)、或其混合物的马来酸酐接枝共聚物。
本文记载的羧基官能化聚合物在润滑剂技术中已知。例如含马来酸酐的酯和苯乙烯的聚合物由美国专利6,544,935已知。接枝的苯乙烯-乙烯-α烯烃聚合物在国际公开WO01/30947中教导。衍生自异丁烯和异戊二烯的共聚物已经用于制备分散剂并且在国际公开WO01/98387中报导。接枝的苯乙烯-丁二烯和苯乙烯-异戊二烯共聚物记载在大量参考文献中，包括DE3,106,959；和美国专利5,512,192、和5,429,758中。聚异丁烯琥珀酸酐已经记载在许多公开文本中，包括美国专利4,234,435；3,172,892；3,215,707；3,361,673；和3,401,118中。接枝的乙烯-丙烯共聚物已经记载在美国专利4,632,769；4,517,104；和4,780,228中。(α烯烃马来酸酐)的酯的共聚物已经记载在美国专利5,670,462中。异丁烯和共轭二烯的共聚物(例如异丁烯-异戊二烯共聚物)已经记载在美国专利7,067,594和7,067,594以及美国专利申请US2007/0293409中。乙烯、丙烯和非共轭二烯(例如双环戊二烯或丁二烯)的三聚物记载在美国专利5,798,420和5,538,651中。典型地，在这一段中提到的包含二烯单体(例如丁二烯或异戊二烯)的聚合物为部分或全部氢化的。许多聚合物主链还记载在“Chemistry andTechnology of Lubricants，第二版，由R.M.Mortier和S.T.Orszulik编辑，由Blackie Academic&Professional出版”中。尤其是页144-180中讨论了许多聚合物主链(i)-(iv)和(vi)-(viii)。
本发明的聚合物主链(除聚异丁烯)可具有这样的数均分子量(通过凝胶渗透色谱法，聚苯乙烯标准)，其可为高达150,000或更高，例如1,000或5,000至150,000、或至120,000或至100,000。合适的数均分子量范围的实例包括10,000-50,000、或6,000-15,000、或30,000-50,000。在一个实施方案中，聚合物主链具有大于5,000的数均分子量，例如大于5000至150,000。上述确定的分子量上下限的其它组合也可预期。当本发明的聚合物主链为聚异丁烯时，其数均分子量(通过凝胶渗透色谱法，聚苯乙烯标准)可为350-15,000、或550-10,000、或500-10,000、或750-5000或750-2500。(因此，聚异丁烯琥珀酸酐可衍生自具有任何上述分子量的聚异丁烯。）某些可商购的聚异丁烯聚合物具有的数均分子量为550、750、950至1000、1550、2000、或2250。一些可商购的聚异丁烯聚合物可通过共混一种或多种不同重量的聚异丁烯聚合物而获得如上所述的数均分子量。在一个实施方案中，羧基官能化聚合物包括数均分子量为约500-约10,000且含至少一个接枝琥珀酸基团(典型地来自聚异丁烯与马来酸酐的反应)的聚异丁烯。
在一个实施方案中，产品可通过使羧基官能化聚合物与具有至少2或3或4个芳基基团、至少一个-NH2官能团、和至少2个仲或叔氨基的胺官能化添加剂反应而获得或得到。具有至少2或3或4个芳基基团的胺官能化添加剂可与羧基官能化聚合物在本领域技术人员熟知的反应条件下反应，以形成羧基官能化聚合物的酰亚胺和/或酰胺。
在某些实施方案中，可通过或通过使羧基官能化聚合物与具有至少2或3或4个芳基基团、至少一个-NH2官能团、和至少2个仲或叔氨基的胺反应获得的胺官能化羧基官能化聚合物可由式(4)和/或(5)表示：
或者
其中，各个变量R1、R2和U独立地如以前所记载。BB表示聚合物主链并且可为聚异丁烯(PIB)、或者(i)氢化烯基芳基共轭二烯共聚物(尤其是苯乙烯-丁二烯的氢化共聚物)、(ii)聚烯烃(尤其是乙烯-α烯烃，例如乙烯-丙烯共聚物)、(iii)氢化异戊二烯聚合物(尤其是氢化苯乙烯-异戊二烯聚合物)、或(iv)异戊二烯和异丁烯的共聚物。BB可被如式(4)和(5)所示的一个琥珀酰亚胺基团取代，或它可被多个琥珀酰亚胺基团取代。在一个实施方案中，BB可为异戊二烯和异丁烯的共聚物。式(4)和(5)中所示的胺结构部分也可被由式(2a)、(3)、(3a)、(3b)、(3c)或其混合物的相应胺结构部分完全或部分取代。
当聚合物主链BB为聚异丁烯时，所得羧基官能化的聚合物通常可为聚异丁烯琥珀酸酐。如式(1)中所定义，w通常可为1-5、或1-3(或在式(1a)中所定义，w可为0-4或0-2)。当BB为非聚异丁烯且在其上接枝马来酸酐(或其它羧酸官能团)时，一个或多个接枝马来酸酐基团可为与一种或多种上述胺反应所形成的琥珀酰亚胺。琥珀酰亚胺基团的数目可为1-40、或2-40、或3-20。
胺官能化的羧基官能化聚合物可通过或通过使衍生自马来酸酐-苯乙烯共聚物、马来酸酐-苯乙烯共聚物的酯、α-烯烃马来酸酐共聚物；或其混合物的羧基官能化聚合物，与具有至少3或4个芳基基团、至少一个-NH2官能团、和至少2个仲或叔氨基的胺反应获得。典型地，这一类型的产物可描述为交替共聚物。在交替共聚物内部，一个或多个马来酸酐衍生的基团可为式(6)表示的基团：
其中R1、R2和U如先前所记载，且式(6)的基团可通过一个或两个在以上琥珀酰亚胺环结构上所示的波状键接连接聚合物主链的其他组分。或者，仅一个波状键可连接聚合物且第二个波状键可连接氢原子或其它非聚合基团。式(6)中的胺衍生基团还可被如上所记载的任何胺，例如式(3)中的胺、或其混合物替换。
作为衍生自聚异丁烯(在式(7)中表示为“PIB”)的邻氨基苯甲酸衍生物的合适结构的实例，邻氨基苯甲酸衍生物和4-氨基二苯基胺可由式(7)表示：
本文中应注意，在其他分散剂中，存在琥珀酰亚胺结构部分到聚异丁烯的各种连接形式，除普通单键外，还包括各种环状连接结构，并且所述结构并不用于限定本发明。
在一个实施方案中，胺官能化的羧基官能化聚合物可衍生自一种芳族胺和非聚异丁烯聚合物主链。衍生自4-氨基二苯基胺的邻氨基苯甲酸衍生物的合适结构的实例可由式(8)表示：
其中如上的BB表示聚合物主链。典型地，BB可为衍生自乙烯-丙烯共聚物的乙烯-丙烯共聚物。如上所示，BB用马来酸酐接枝并且官能化形成酰亚胺基团，且u为接枝在主链的不同位置上的方括号内所示的接枝单元的数目。典型地u可为1-2000、1-500、1-250、1-50、1-20、1-10、或1-4。
胺官能化羧基官能化聚合物的更详细说明发现在国际申请PCT/US2008/082944中。尤其是参见[0013]-[0021]、[0027]-[0091]段和[0111]-[0135]段中公开的制备例1-25。
如果羧基官能化聚合物与包含羟基的芳族化合物反应，由此芳基基团可通过酯键连接聚合物。含羟基的芳族化合物可具有直接位于芳族环上的羟基，从而为苯氧基、或者它可位于随后连接芳基的基团上，从而为醇羟基。芳族化合物可包含至少2、3、或4个芳族环。环可为如上所述的任何类型的芳族环并且可包括稠环芳族化合物。还可使用聚合或低聚芳族化合物。在一个实施方案中，产物可通过使羧基官能化聚合物与具有2或更多个芳基基团的羟基官能化添加剂反应而获得或得到，如在2006年8月24日Bera等人的美国专利公开2006-0189492中记载的，例如参见段落0122。这种材料可由下式表示：
其中PIB表示聚异丁烯且n为2-24。
上文所述类型的多种聚合分散剂可组合使用，例如基于不同聚合主链的分散剂(例如聚异丁烯主链以及基于烯烃共聚物主链的那些)的混合物，以及无论在相同或不同聚合物主链上，具有在其上缩合的不同类型芳族材料的分散剂。从而，例如，分散剂组分可包括(i)数均分子量为约500-约10,000的含至少一个琥珀酸酐基团(任选地，每聚合物，平均到组合物)的聚异丁烯，其与具有至少3个芳族环和至少一个伯或仲氨基的芳族胺缩合以及(ii)含多个羧基(任选地，每聚合物，平均到组合物)的烯烃共聚物与硝基取代的芳族胺的缩合产物。在一个实施方案中，琥珀酸酐基团或分散剂的聚合物基团上的其它羧基的数目可表示为“每聚合物，平均到组合物”。当这样表示时，聚合物的任何未反应的部分，即未用琥珀酸酐或其它羧基官能化，归入统计内。在另一个实施方案中，这种基团在分散剂的聚合物基团上的数目可通过从计算中排除任何未官能化(未反应的)聚合物链来计算。计算的后一模式旨在用于没有术语“每聚合物，平均到组合物”的情况下。可使用任一表征。
聚合分散剂在完全配制的润滑剂中的量可为至少0.2或0.3重量%，例如0.3-5%或0.5-3%或1-2%。或者，如果聚合分散剂作为浓缩物提供，分散剂在该浓缩物中的量将相应地更高，例如2-30%或5-20%。
所公开技术的组合物还包括油溶钛化合物，当使用时，其可例如在发动机油中用来赋予例如沉积控制、氧化性、和可滤性有益的效果的性能。“油溶性”或“烃溶性”是指以宏观或大致规模(gross scale)溶解或分散在油或烃(视情况而定，典型地为矿物油)中，从而可制备适用的溶液或分散体。为了制备可用的润滑剂配制剂，钛材料不应在数天或数周内沉淀或沉降出来。这种材料可在分子规模上显示真实可溶性，或可能以各种尺寸或规模的聚结形式存在，前提是它们已经在大致规模上溶解或分散。
油溶含钛材料的性质可以不同。可以使用的各种材料，制备它们的方法公开在2010年6月1日Brown等人的美国专利7,727,943中。可用在所公开技术中的钛化合物为各种有机的含Ti(IV)化合物，例如醇钛(IV)，包括甲醇钛、乙醇钛、丙醇钛、异丙醇钛、丁醇钛、和2-乙基己醇钛；和其它钛化合物或配合物，包括但不限于酚钛；羧酸钛，例如2-乙基-1-3-己二酸钛(IV)或柠檬酸钛或油酸钛或酒石酸钛；和(三乙醇胺合)异丙醇钛(IV)。油溶性钛的其他形式包括磷酸钛，例如二硫代磷酸钛(例如二烷基二硫代磷酸盐)和磺酸钛(例如烷基磺酸盐)，或通常，钛化合物与各种酸材料反应形成盐，特别是油溶性盐的反应产物。因此，钛化合物尤其可衍生自有机酸、醇、和二醇。Ti化合物还可以以含有Ti-O-Ti结构的二聚或低聚形式存在。这种钛材料可商购或可通过本领域技术人员显而易见的合适的合成技术而容易制得。它们在室温下可以作为固体或液体存在，取决于具体的化合物。它们还可以以在适当惰性溶剂中的溶液形式提供。
在另一个实施方案中，钛可作为Ti改性的分散剂，例如琥珀酰亚胺分散剂提供。这种材料可通过在钛源例如醇钛和烃基取代的琥珀酸酐(例如烯基(或烷基)琥珀酸酐)之间形成钛混合酐来制备。所得钛酸酯-琥珀酸酯中间体可直接使用，或可与下述许多材料中的任一种反应，例如(a)具有游离、可缩合的-NH官能团的基于聚胺的琥珀酰亚胺/酰胺分散剂；(b)基于聚胺的琥珀酰亚胺/酰胺分散剂的组分，即烯基-(或烷基-)琥珀酸酐和聚胺、(c)通过取代的琥珀酸酐与多元醇、氨基醇、聚胺、或其混合物反应而制备的含羟基聚酯分散剂。或者，该钛酸酯-琥珀酸酯中间体可与其它试剂，例如醇、氨基醇、醚醇、聚醚醇或多元醇，或者脂肪酸反应，并且其产物或者直接使用为润滑剂提供Ti，或者进一步与如上所述的琥珀酸分散剂反应。例如，1(摩尔)份钛酸四异丙基酯可与2(摩尔)份聚异丁烯取代的琥珀酸酐在140-150°C下反应5-6小时，以提供钛改性的分散剂或中间体。所得材料(30g)可进一步与来自聚异丁烯取代的琥珀酸酐和聚亚乙基多胺混合物的琥珀酰亚胺分散剂(127g+稀释油)在150°C下反应1.5小时，以生产钛改性的琥珀酰亚胺分散剂。在某些实施方案中，钛化合物例如Ti羧酸盐(例如柠檬酸盐、酒石酸盐)可与分散剂反应或结合。如此处理可改进Ti化合物的可溶性。
在一个实施方案中，油溶性钛化合物可包括醇钛(IV)或羧酸钛(IV)。合适的醇盐为异辛醇钛(IV)或其他醇盐，其中烷氧基可包含3-20个碳原子或4-15、6-12、或8个碳原子。烷氧基可为直链或支化。合适的羧酸盐为新癸酸钛(IV)或其它羧酸盐，其中羧酸盐基团可包含3-20个碳原子、4-18、6-16、8-12、或10个碳原子。羧酸盐基团可为支化或直链。
油溶性钛化合物可在润滑剂组合物中存在以提供5-10,000、或-5000或-1000份每百万重量份(ppm)的钛的量存在，或者10-500ppm或20-400ppm或50-200ppm。在其它实施方案中，钛的量可为5-45ppm。据信，甚至在相对较低的钛浓度下，例如5-100或8-50或8-45或10-45或15-30或10-25ppm的钛或1至小于50ppm、或8至小于50ppm重量Ti，也可获得清洁/防污/抗氧化益处，而不考虑化合物的阴离子部分。据信超过50或70或100ppm的量也为有效。
可以以任何便利方式将钛化合物赋予润滑剂组合物中，例如通过加入若非如此为成品的润滑剂(最终处理)中，或通过将钛化合物以浓缩物形式预混在油或其他合适的溶剂中，任选与一种或多种附加组分一起，例如抗氧化剂、摩擦改性剂例如甘油单油酸酯、分散剂例如琥珀酰亚胺分散剂、或清净剂例如高碱性硫化酚盐清净剂。这种附加组分，通常与稀释油一起，可通常包含在添加剂预配料(package)、有时还称为DI(清净剂-抑制剂)预配料中。
附加的常规组分可用于制备本发明的润滑剂，例如通常在曲轴箱润滑剂中使用的那些添加剂。曲轴箱润滑剂通常可包含下文所述的任一或所有下列组分。一种这样的添加剂为除如上所述缩合产物之外的无灰分散剂或聚合分散剂，即除羧基官能化的聚合物与芳族结构部分的缩合产物之外的。分散剂在润滑剂领域为大家所熟知并且主要包括称为无灰分散剂和聚合分散剂的那些。无灰分散剂这样称是因为，以提供其的形式，其不包含金属且当加入润滑剂时，因而通常不对硫酸盐灰份做出贡献。然而，一旦将其加入包括含金属物质的润滑剂时，毫无疑问其可能与四周的金属相互作用。无灰分散剂的特征在于极性基团连接至较高分子量的烃链。典型的无灰分散剂包括具有各种化学结构的N-取代长链烯基琥珀酰亚胺，通常包括
其中R1各自独立地为烷基，通常为基于聚异丁烯前体的分子量(Mn)为500-5000的聚异丁烯基团，且R2为亚烷基基团，通常为乙烯基(C2H4)。当x为1时，分子的胺衍生部分可对应于二亚乙基三胺；当x为2时，三亚乙基四胺；当x为3时，四亚乙基五胺。x的值可为1-8或2-6或3-4。这种分子通常衍生自烯基酰化剂与聚胺的反应，并且除了如上所示的普通酰亚胺结构以外，在这两个结构部分之间的各种键合也是可能的，包括各种酰胺和季铵盐。同时，在酰亚胺结构上的R1基团的各种键合模式可用，包括各种环键。酰化剂的羰基对胺的氮原子的比率可为1:0.5-1:3，且在其它情况下为1:1-1:2.75或1:1.5-1:2.5。这些材料中的某些还可被称作烃基取代的琥珀酸酐或其反应性等同物与聚(亚烷基胺)的缩合产物。琥珀酰亚胺分散剂更充分地记载在美国专利4,234,435和3,172,892以及EP0355895中。这些分散剂可能与如上所述的那些相似，除了它们通常不包含芳族结构部分外。
另一种无灰分散剂为高分子量酯。这些材料与如上所述的琥珀酰亚胺相似，除了它们可能被看作通过使烃基酰化剂和多元脂族醇例如丙三醇、季戊四醇或山梨糖醇反应而制备。这种材料更详细地记载在美国专利3,381,022中。
另一种无灰分散剂为曼尼希碱。这些为通过较高分子量、烷基取代的酚、亚烷基聚胺、和醛例如甲醛缩合而形成。这种材料可具有以下通用结构：
(包含各种异构体等)并且更详细地记载在美国专利3,634,515中。
其它分散剂包括聚合分散添加剂，其通常为基于烃的包含赋予聚合物分散特性的极性官能团的聚合物。这些再一次可能与如上公开技术的分散剂相似，除了它们通常不包含所需的芳族组分。
分散剂还可通过与任何各种试剂反应进行后处理。在这些之中，为脲、硫脲、二巯基噻二唑、二硫化碳、醛、酮、羧酸、烃取代的琥珀酸酐、腈、环氧化物、硼化合物、和磷化合物。详细描述此类处理的参考文献列在美国专利4,654,403中。
如果存在，这种其他或附加分散剂的量可为润滑剂的0.1-8重量%、0.5-5%、1-4%、或2-3%。
可存在的另一种添加剂为清净剂，通常为含金属的清净剂。用于发动机润滑领域中的最常规清净剂向润滑剂提供碱性或TBN，由于存在碱性金属化合物(金属氢氧化物、氧化物、或碳酸盐，通常基于如钙、镁、或钠的金属)。这种金属高碱性清净剂，也称为高碱性或超碱性盐，通常为单相、均匀的牛顿体系，其特征为金属含量超过根据金属和与金属起反应的特定酸性有机化合物的化学计量用于中和而存在的那些。过量金属的量通常以术语金属比表示。术语“金属比”是金属的总当量与酸性有机化合物当量的比值。中性金属盐的金属比为1。金属含量是正盐中存在金属的4.5倍的盐具有3.5当量金属过量，或其金属比为4.5。在一个实施方案中，润滑剂组合物可包括金属比为至少3、至少5、至少8、或至少10且例如至多20或15或12或10的高碱性清净剂。
高碱性材料通常通过使酸性物质(一般为无机酸或低级羧酸例如二氧化碳)与酸性有机化合物(也称为基质)、化学计量过量的金属碱，通常在一种用于酸性有机基质的惰性有机溶剂(例如矿物油、石脑油、甲苯、二甲苯)的反应介质中反应而制备。任选存在少量促进剂例如酚或醇。酸性有机基质通常具有足够数目的碳原子，以提供在油中的溶解度。
酸性有机基质可包括磺酸，例如提供磺酸盐清净剂的烃基取代的苯磺酸、提供羧酸盐清净剂的羧酸(一种水杨酸盐清净剂)、提供酚盐清净剂的酚或硫桥接的酚、或提供膦酸盐清净剂的膦酸。其他类型的清净剂包括salixarate和水杨醇清净剂。这种高碱性材料以及它们的方法或制备为本领域技术人员所熟知。描述用于制备磺酸、羧酸、酚、膦酸的碱性金属盐、及这些物质中任意两种或更多种的混合物的技术的专利包括美国专利2,501,731；2,616,905；2,616,911；2,616,925；2,777,874；3,256,186；3,384,585；3,365,396；3,320,162；3,318,809；3,488,284；和3,629,109。Salixarate清净剂记载在美国专利6,200,936和PCT公开WO01/56968中。水杨醇清净剂记载在美国专利6,310,009中。在某些实施方案中，清净剂可包括高碱性硫化酚盐清净剂，其可以0.1-2重量%或0.2-1%或0.4-0.8%的量存在。在某些实施方案中，清净剂可包括磺酸盐清净剂，其可以0.1-2重量%或0.2-1%或0.5-0.9%的量存在。在某些实施方案中，可存在硫化酚盐清净剂和磺酸盐清净剂两者，以0.2-4重量%、或0.5-2.5%或1.0-1.5%的总量存在。
另一种组分可为抗氧化剂。抗氧化剂包括酚抗氧剂，其可包括包含2或3个叔丁基基团的丁基取代酚。该对位还可被烃基或桥连两个芳族环的基团占据。后一抗氧化剂更详细地记载在美国专利6,559,105中。特定的和有用种类的酚类抗氧剂为受阻酚酯，其可具有以下通用结构
其中R3为烃基，例如包含如1-18或2-12或2-8或2-6个碳原子，例如4或8个碳原子的烷基；且叔烷基可为叔丁基。这种抗氧化剂及其制备更详细地记载在美国专利6,559,105中。
抗氧化剂还包括芳族胺，例如烷基化二苯基胺和烷基化苯基萘基胺，包括苯基-α-萘胺(“PANA”)和烷基化PANA。典型的烷基化二苯基胺包括壬基化二苯基胺。如本文记载的芳族胺抗氧化剂一般而言为非聚合抗氧化剂，与如上所记载技术的包含聚合芳族材料不同，其中一些可能呈现某些抗氧化剂活性。其它抗氧化剂包括硫化烯烃、钛化合物、和钼化合物。例如美国专利4,285,822公开了含钼的润滑油组合物和含硫组合物。美国专利申请公开2006-0217271公开了各种钛化合物，包括醇钛和钛酸酯分散剂，这些材料还可赋予沉积控制和可滤性的改进。毫无疑问，抗氧化剂的常用量将取决于特定的抗氧化剂及其各自的效力，但是说明性的总量可为0.01-5重量%或0.05-3%或0.1-1%或0.2-0.5%或0.15-4.5%或0.2-4%。另外，可存在超过一种抗氧化剂，并且这些的某些组合可能在它们的组合总体效果方面有协同效果。
粘度改进剂(有时也称为粘度指数改进剂或粘度改性剂)可包括在这一技术的组合物中。粘度改进剂通常为聚合物，包括聚异丁烯、聚甲基丙烯酸酯、氢化二烯聚合物、聚烷基苯乙烯、酯化的苯乙烯-马来酸酐共聚物、氢化的链烯基芳烃-共轭二烯共聚物、和聚烯烃。也具有分散剂和/或氧化稳定性能的多官能粘度改进剂为已知并且可任选使用。
另一种可用的添加剂为抗磨剂。抗磨剂的实例包括含磷抗磨/极压剂，例如金属硫代磷酸盐、磷酸酯及其盐、含磷羧酸、酯、醚、和酰胺；以及亚磷酸盐。在某些实施方案中，磷抗磨剂可以提供0.01-0.2或0.015-0.15或0.02-0.1或0.025-0.08%磷的量存在。抗磨剂通常为二烷基二硫代磷酸锌(ZDP)。对于典型的ZDP，其可包含11%的P(基于无油计算)，合适的量可包括0.09-0.82或-1.0%。不含磷的抗磨剂包括硼酸酯(包括硼酸化的环氧化物)、二硫代氨基甲酸盐化合物、含钼化合物、和硫化烯烃。
其他种类的抗磨剂包括酒石酸酯，酒石酰胺、和酒石酰亚胺，例如油烯基酒石酸酰亚胺、以及广义的羟基-多元羧酸的酯、酰胺、和酰亚胺。这些材料还可赋予润滑剂抗磨损性能之外的其他功能。这些材料更详细地记载在美国公开2006-0079413、PCT公开WO2010/077630中。
润滑剂还可包含含磷酸(phorphorus acid)的金属盐。式[(R8O)(R9O)P(=S)-S]n-M的金属盐，其中R8和R9独立地为含3-30个碳原子的烃基，可以容易地通过加热五硫化二磷(P2S5)和醇或酚形成O,O-二烃基二硫代磷酸获得。反应提供R8和R9基团的醇可为醇的混合物，例如异丙醇和4-甲基-2-戊醇的混合物，并且在某些实施方案中为仲醇和伯醇的混合物，例如异丙醇和2-乙基己醇。所得酸可与碱性金属化合物反应形成盐。具有n价的金属M通常为铝、铅、锡、锰、钴、镍、锌或铜，并且在多数情况下为锌，以形成二烷基二硫代磷酸锌。这种材料为众所周知并且对于润滑剂配制剂领域的技术人员可易于获得。对于在发动机中提供良好磷保留申请合适的方案例如公开在美国公开申请2008-0015129中，例如参见权利要求。
可在润滑油中任选使用的其他添加剂包括倾点下降剂、极压剂、抗磨剂、颜色稳定剂和消泡剂。
众所周知如上所述的一些材料在最终配制剂中可互相影响，以便最终配制剂的组分可不同于最初添加的那些。例如，金属离子(例如为清净剂的)可迁移至其它分子的其它酸性或阴离子位点。由此形成的产物，包括以其预期的用途使用本发明的组合物时形成的产物，可能难以容易地说明。然而，所有这类改性和反应产物包括在本发明的范围内；本发明包括通过混合如上所述组分制备的组合物。
本文记载的润滑剂可通过将润滑剂供入装置而用于润滑机械装置。该装置可为内燃机，例如汽油燃料或柴油燃料汽车发动机、重型柴油机、船用柴油机、或固定燃气发动机。这种发动机可为油底壳润滑的，并且润滑剂可从其可能润滑发动机运动部件的地方提供至油底壳。或者，润滑剂可由非油底壳部分的不同来源提供。
实施例
制备一系列包含以下组分的润滑剂配制剂，以重量%表示：
2.19%高碱性磺酸钙和苯酚盐清净剂(包括约40%稀释油)
1.1%二烷基二硫代磷酸锌(包括9%油)
1.5%分散剂粘度改性剂，包含芳族氮化合物组分(包括66.5%稀释油)
0.5%受阻酚酯抗氧化剂
0.3%芳族胺抗氧化剂
0.1%烃基取代的琥珀酸酐
较少量的腐蚀抑制剂和消泡剂
附加组分-见下文
具有润滑粘度的基础油-第II类基础油，其量至=100%
通过与上述组分一起包括以所标量的下表中所列的那些材料制备6种特定的润滑剂配制剂。对各个润滑剂配制剂通过ACEA E-5加压差示扫描量热法进行氧化诱导时间测试。在这一测试中，在被提供压缩空气、能够加压至700kPa(100psi)的压力池中加热润滑剂样品。在50°C下平衡之后，使温度以40°C/min升至210°C并且在210°C下保持直到通过热流检测到氧化发生。氧化诱导时间为从达到100°C时开始，直到氧化开始的时间。结果记录为氧化开始的分钟数。时间越长表明稳定性越高。
在上表中，实施例C1-C5为对比例或对照例。来自芳族胺的琥珀酰亚胺分散剂为聚异丁烯取代的琥珀酰亚胺与芳族胺的缩合产物，所述芳族胺包括大部分被认为具有上式(2)的结构，包括其异构体的分子。在润滑剂中使用提供100ppm Ti的量的四(2-乙基己基)钛酸酯。
结果表明有或无芳族琥珀酰亚胺分散剂或基于聚(乙烯基胺)的琥珀酰亚胺分散剂对于氧化稳定性影响非常小(对比例C1、C2和C3)。向C1和C2的润滑剂中加入100ppm可溶性钛导致约41-49%的稳定性的适度增加，就OIT而言(将C4与C1以及C5与C2比较)。然而，当将100ppm钛加入还包含芳族琥珀酰亚胺分散剂的润滑剂时，OIT增加超过70%至超过160分钟的值(将实施例6与C2比较)。这表示氧化稳定性的显著和预料不到的改进。
以上参考的各文献引入本文供参考。提及任何文件不是承认该文件有资格作为现有技术或构成以任何权限的本领域技术人员的公知常识。除在实施例中外，或者其中另外明确标明，本说明书中所有规定材料量、反应条件、分子量、碳原子数量等的数值量，将理解为通过词“约”限定。应该理解的是，本文提出的上限和下限的量、范围和比例可独立地组合。类似地，本发明的各要素的范围和量可与任何其他要素的范围或量一起使用。本文中所用的术语“基本由......构成”允许包括不会实质影响所述组合物的基本和新颖的特性的物质。
Claims (13)
1.一种润滑剂组合物，其包含
(a)具有润滑粘度的油；
(b)0.2-5重量％的分散剂，其包含羧基官能化聚合物经由酰胺或酰亚胺与芳族结构部分的缩合产物，其中分散剂包含与具有至少3个芳族环和至少一个伯或仲氨基的芳族胺的缩合产物；和
(c)油溶性钛化合物，其中油溶性钛化合物以提供以重量计每百万份5-10,000份钛的量存在。
2.根据权利要求1的润滑剂组合物，其中所述芳族胺由以下结构表示：
其中各变量独立地
R1和R2为氢或C1-5烷基；
U为脂基、脂环基或芳基；且
w为0-9。
3.根据权利要求1或2的润滑剂组合物，其中分散剂包含与硝基取代的芳族胺的缩合产物。
4.根据权利要求1或2的润滑剂组合物，其中羧基官能化聚合物包括数均分子量为500-10,000且含至少一个琥珀酸酐基团的聚异丁烯结构部分。
5.根据权利要求1或2的润滑剂组合物，其中分散剂(b)包括(i)数均分子量为500-10,000的含至少一个琥珀酸酐基团的聚异丁烯结构部分，其与具有至少3个芳族环和至少一个伯或仲氨基的芳族胺缩合，以及(ii)含多个羧基的烯烃共聚物与硝基取代的芳族胺的缩合产物。
6.根据权利要求1或2的润滑剂组合物，其中油溶性钛化合物包括醇钛(IV)或羧酸钛(IV)。
7.根据权利要求1或2的润滑剂组合物，其中油溶性钛化合物包括2-乙基己醇钛(IV)。
8.根据权利要求1或2的润滑剂组合物，其中油溶性钛化合物包括新癸酸钛。
9.根据权利要求1或2的润滑剂组合物，其中除羧基官能化聚合物与芳族结构部分的缩合产物外，进一步包括0.5-5重量％的无灰分散剂或聚合分散剂。
10.根据权利要求1或2的润滑剂组合物，其中进一步包括0.05-3重量％的非聚合芳族胺抗氧剂。
11.根据权利要求1或2的润滑剂组合物，其中进一步包括至少一种选自粘度改进剂、倾点下降剂、含金属清净剂、二烷基二硫代氨基甲酸锌、和抗磨剂的添加剂。
12.一种润滑机械装置的方法，包括将权利要求1-11中任一项的润滑剂组合物供入所述装置中。
13.一种改进用于机械装置的润滑剂氧化稳定性的方法，包括在所述润滑剂中包含(b)0.2-5重量％的分散剂，其包含羧基官能化聚合物经由酰胺或酰亚胺与芳族结构部分的缩合产物，其中分散剂包含与具有至少3个芳族环和至少一个伯或仲氨基的芳族胺的缩合产物；和(c)油溶性钛化合物，其中油溶性钛化合物以提供以重量计每百万份5-10,000份钛的量存在。
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| CN107235856A (zh) * | 2017-06-22 | 2017-10-10 | 新乡市瑞丰新材料股份有限公司 | 一种胺类化合物、润滑油用胺类无灰分散剂及其制备方法 |
| CN107162927A (zh) * | 2017-06-22 | 2017-09-15 | 新乡市瑞丰新材料股份有限公司 | 一种胺类化合物、润滑油用胺类无灰分散剂及其制备方法 |
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| CA2809310A1 (en) | 2012-03-01 |
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