CN112392595B - 减少船用柴油机中的活塞沉积物的方法 - Google Patents
减少船用柴油机中的活塞沉积物的方法 Download PDFInfo
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- CN112392595B CN112392595B CN202010810896.5A CN202010810896A CN112392595B CN 112392595 B CN112392595 B CN 112392595B CN 202010810896 A CN202010810896 A CN 202010810896A CN 112392595 B CN112392595 B CN 112392595B
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- 229940116351 sebacate Drugs 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000003333 secondary alcohols Chemical class 0.000 description 1
- 239000003079 shale oil Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 238000000629 steam reforming Methods 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- JZALLXAUNPOCEU-UHFFFAOYSA-N tetradecylbenzene Chemical compound CCCCCCCCCCCCCCC1=CC=CC=C1 JZALLXAUNPOCEU-UHFFFAOYSA-N 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- MQHSFMJHURNQIE-UHFFFAOYSA-N tetrakis(2-ethylhexyl) silicate Chemical compound CCCCC(CC)CO[Si](OCC(CC)CCCC)(OCC(CC)CCCC)OCC(CC)CCCC MQHSFMJHURNQIE-UHFFFAOYSA-N 0.000 description 1
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 description 1
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 description 1
- 150000004867 thiadiazoles Chemical class 0.000 description 1
- 125000000464 thioxo group Chemical group S=* 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 125000002469 tricosyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- ZAGXLQIHXTXRFW-UHFFFAOYSA-N tris(2-ethyl-4-methylhexyl)-tris(2-ethyl-4-methylhexyl)silyloxysilane Chemical compound CCC(C)CC(CC)C[Si](CC(CC)CC(C)CC)(CC(CC)CC(C)CC)O[Si](CC(CC)CC(C)CC)(CC(CC)CC(C)CC)CC(CC)CC(C)CC ZAGXLQIHXTXRFW-UHFFFAOYSA-N 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02B—INTERNAL-COMBUSTION PISTON ENGINES; COMBUSTION ENGINES IN GENERAL
- F02B77/00—Component parts, details or accessories, not otherwise provided for
- F02B77/04—Cleaning of, preventing corrosion or erosion in, or preventing unwanted deposits in, combustion engines
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/04—Use of additives to fuels or fires for particular purposes for minimising corrosion or incrustation
-
- 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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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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
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
- C10M169/045—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution and non-macromolecular compounds
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
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- C10L1/14—Organic compounds
- C10L1/143—Organic compounds mixtures of organic macromolecular compounds with organic non-macromolecular compounds
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- C10L1/16—Hydrocarbons
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- C10L10/00—Use of additives to fuels or fires for particular purposes
- C10L10/06—Use of additives to fuels or fires for particular purposes for facilitating soot removal
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M129/50—Carboxylic acids; Salts thereof having carboxyl groups bound to a carbon atom of a six-membered aromatic ring monocarboxylic
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- C10M145/10—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing monomers having an unsaturated radical bound to a carboxyl radical, e.g. acrylate
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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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
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01M—LUBRICATING OF MACHINES OR ENGINES IN GENERAL; LUBRICATING INTERNAL COMBUSTION ENGINES; CRANKCASE VENTILATING
- F01M11/00—Component parts, details or accessories, not provided for in, or of interest apart from, groups F01M1/00 - F01M9/00
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F02—COMBUSTION ENGINES; HOT-GAS OR COMBUSTION-PRODUCT ENGINE PLANTS
- F02B—INTERNAL-COMBUSTION PISTON ENGINES; COMBUSTION ENGINES IN GENERAL
- F02B77/00—Component parts, details or accessories, not otherwise provided for
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L2270/00—Specifically adapted fuels
- C10L2270/02—Specifically adapted fuels for internal combustion engines
- C10L2270/026—Specifically adapted fuels for internal combustion engines for diesel engines, e.g. automobiles, stationary, marine
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
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- C10M2203/1025—Aliphatic fractions used as base material
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2207/00—Organic non-macromolecular hydrocarbon compounds containing hydrogen, carbon and oxygen as ingredients in lubricant compositions
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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
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Abstract
一种在用符合船用残渣燃料的ISO 8217 2017燃料标准并具有大于0.1质量%和小于0.5质量%的硫含量的船用残渣燃料作为燃料的四冲程船用柴油机的运行过程中减少发动机活塞上的沉积物发生率的方法。所述方法包括使用一种润滑油组合物润滑发动机,所述润滑油组合物包含:(a)基于组合物质量计至少50质量%的具有润滑粘度的油;(b)基于组合物质量计5至25质量%的油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物;(c)基于组合物质量计0.1至10质量%的一种或多种油溶性或油分散性无灰分散剂;和任选地,(d)基于组合物质量计0.1至10质量%的聚烯取代的琥珀酸酐。
Description
本发明涉及一种减少发动机中的活塞沉积物的方法,特别涉及一种减少用具有低硫浓度的船用残渣燃料(marine residual fuel)作为燃料的四冲程船用柴油机的活塞上的沉积物发生率的方法。
目前,用于为在近海区域运营的航运业中使用的船用柴油机供能的残渣燃料必须具有基于燃料质量计不超过3.5质量%的硫含量。但是,与其它运输行业相同,存在减少由商业和休闲航运造成的有害排放物的环境压力。残渣燃料中存在的硫是环境污染的主要成因。自2015年1月以来,世界各地已引入排放控制区(Emission Control Areas)(ECAs),主要是在沿海地区。在这些ECAs,只有当船用燃料具有不超过0.1质量%的硫含量时船舶才可以燃烧它们。ECA准许的燃料相对昂贵,因此强制近海航运也使用它们会在经济上损害全球航运业。取而代之地,国际海事组织(IMO)已经规定了近海航运所用的残渣燃料的硫含量在全球降低到基于燃料质量计不超过0.5质量%。硫含量的这一上限在2020年1月1日生效。
IMO的新法规(被称为IMO 2020)对船主和经营人以及对燃料精炼商和生产商都带来了问题。对于船主,面临着选择。船舶必须一开始就用较低硫含量的燃料运行,或者,可继续使用现有的较高硫含量(<3.5质量%)燃料,条件是采取措施除去其燃烧造成的大气污染物。后一选项涉及使用能从排气中除去超过95%的硫氧化物和大部分颗粒物的排气净化系统(通常被称为“洗涤器”)。但是购买和安装洗涤器以及在安装升级设备时船舶的不可用性对船主而言都是相当大的财务成本。一些船主和经营人会发现改装他们的船舶以能够继续使用较高硫含量的燃料更有商业吸引力,而对于另一些人,换成较低硫含量的残渣燃料更成本有效。这对燃料精炼商和生产商具有连锁效应。直到IMO法规规定后,才有生产硫含量不超过0.5质量%的残渣燃料的商业动机,因此目前,这样的燃料还未上市。
在2020年1月1日后,这些燃料将有市场,但是市场规模取决于决定使用新燃料的船主和经营人和选择安装洗涤器的其余船主和经营人的比例。燃料精炼商和生产商必须决定低硫含量的残渣燃料的需求有多大和他们要顺应IMO法规生产的燃料的确切类型。有许多不同的方式生产合规的残渣燃料,例如通过使用各种炼油厂料流的组合,它们视必要合适地处理以降低硫含量。新型燃料还必须满足关于船用残渣燃料的现有国际标准规范ISO8217 2017,其规定了各种类别的船用残渣燃料的性质,如最大运动粘度、密度、闪点等。本发明涉及用既满足船用残渣燃料的ISO 8217 2017规范又具有不超过0.5质量%的硫含量的残渣燃料作为燃料的发动机。ISO 8217 2017也规定了船用馏分燃料的国际标准,但这些与本发明无关。
该新型较低硫含量的残渣燃料还要求改变用于润滑船用柴油机的润滑剂。传统上,润滑剂制造商已将他们的产品配制成与具有较高硫含量的燃料一起工作。这样的燃料在燃烧时产生相当大量的硫氧化物,以导致大量酸性物类积聚在润滑剂中。润滑剂因此含有能够中和这些酸以防止发动机部件腐蚀和润滑剂降解的化学物类。颗粒物和碳烟水平也相对较高,因此能将这些分散在润滑剂中的物类是必要的。
即将到来的转向较低硫含量燃料的趋势因此对润滑剂配制者提出新的挑战。为润滑以高硫含量燃料作为燃料的发动机而设计的润滑剂在以该新型燃料作为燃料的相同发动机中没有表现出最佳性能。
关于为润滑以高硫含量船用残渣燃料作为燃料的发动机设计的润滑剂的过往经验表明,在为了中和酸性燃烧产物而必须存在的高碱性金属清净剂存在下,无灰分散剂对活塞清洁度具有负面影响。这归因于润滑剂处理在高硫含量船用残渣燃料中总是存在的沥青质的能力下降,并在台架试验和实机试验中都已观察到。因此到目前为止无灰分散剂在为润滑以高硫含量船用残渣燃料作为燃料的发动机设计的润滑剂中的应用受到限制。
符合IMO 2020法规的新型船用残渣燃料具有降低的硫含量但仍含有沥青质,因为用于除硫的工艺通常不会也除去沥青质。基于过往经验,可能原本预计,在用这些低硫含量燃料运行的发动机中使用的润滑剂中包括无灰分散剂将会类似地导致活塞清洁度不佳。但是令人惊讶地,本发明发明人已经发现,在用于润滑以符合IMO 2020法规(和船用残渣燃料的ISO 8217 2017规范)的船用残渣燃料作为燃料的发动机的润滑剂中,金属清净剂和无灰分散剂的组合实际上导致与不含任何无灰分散剂的类似润滑剂相比活塞沉积物减少。此外,已经发现,可将某些化合物添加到金属清净剂和无灰分散剂的组合中以“增进”这一效应并因此提供进一步增强的活塞清洁度。
相应地,在第一个方面中,本发明提供一种在用符合船用残渣燃料的ISO 82172017燃料标准并具有基于燃料质量计大于0.1质量%和小于0.5质量%的硫含量的船用残渣燃料作为燃料的四冲程船用柴油机的运行过程中减少发动机活塞上的沉积物发生率的方法,所述方法包括使用一种润滑油组合物润滑发动机,所述润滑油组合物包含:
(a)基于组合物质量计至少50质量%的具有润滑粘度的油;
(b)基于组合物质量计5至25质量%的油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物,所述或各油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂具有通过ASTM D2896测得的0至500mg KOH/g的总碱值(TBN);
(c)基于组合物质量计0.1至10质量%的一种或多种油溶性或油分散性无灰分散剂;和任选地,
(d)基于组合物质量计0.1至10质量%的聚烯取代的琥珀酸酐。
优选地,油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物以基于组合物的总质量计6至20质量%,更优选基于组合物的总质量计7至15质量%的量存在。当使用两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物时,这些量是指存在于组合物中的该混合物的质量百分比。
所述方法涉及用符合船用残渣燃料的ISO 8217 2017燃料标准并具有基于燃料质量计大于0.1质量%和小于0.5质量%的硫含量的船用残渣燃料作为四冲程船用柴油机的燃料。符合这些标准的任何残渣燃料适用于进行所要求保护的发明的方法,但优选地,船用残渣燃料包含选自下组的一种残渣炼油厂料流或两种或更多种的混合物:常压塔底油、真空塔底油、轻循环油、重循环油、流体催化裂化循环油、流体催化裂化油浆、热裂化渣油、热焦油、未稀释焦油(unfluxed tar)、热裂化重质馏分油、I类疏松蜡、脱沥青油、热裂化煤油气制液(gas-to-liquid)蜡、加氢精制的轻循环油、加氢精制的重循环油、加氢精制的流体催化裂化循环油、加氢精制的热裂化重质馏分油、加氢精制的塔底油、加氢裂化器蜡乳液(hydrowax)和加氢精制的加氢裂化器脱沥青油。优选地,船用残渣燃料包含两种或更多种这些残渣炼油厂料流的混合物。
更优选地,船用残渣燃料基本由选自下组的一种残渣炼油厂料流或两种或更多种的混合物组成:常压塔底油、真空塔底油、轻循环油、重循环油、流体催化裂化循环油、流体催化裂化油浆、热裂化渣油、热焦油、未稀释焦油(unfluxed tar)、热裂化重质馏分油、I类疏松蜡、脱沥青油、热裂化煤油气制液(gas-to-liquid)蜡、加氢精制的轻循环油、加氢精制的重循环油、加氢精制的流体催化裂化循环油、加氢精制的热裂化重质馏分油、加氢精制的塔底油、加氢裂化器蜡乳液(hydrowax)和加氢精制的加氢裂化器脱沥青油。更优选地,船用残渣燃料基本由两种或更多种这些残渣炼油厂料流的混合物组成。
符合IMO 2020的燃料必须符合船用残渣燃料的ISO 8217 2017燃料标准并具有所要求的低硫含量,但组成和物理性质可变,取决于其生产中使用的残渣料流。选择使用哪些掺合组分涉及复杂的计算,基于的因素包括可得性、成本、相容性和稳定性影响和炼油厂设计在内。
润滑油组合物包含(b)油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物。这样的清净剂是本领域中已知的。
清净剂是减少发动机中的活塞沉积物(例如高温清漆和亮漆沉积物)形成的添加剂;其通常具有酸中和性质并能使细碎固体保持悬浮。大多数清净剂基于“皂”,即酸性有机化合物的金属盐。相应地,本发明的润滑油组合物包括水杨酸的碱金属或碱土金属盐作为皂,即水杨酸皂。
优选地,油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物为润滑油组合物提供30至100,优选40至90,更优选50至80毫摩尔水杨酸皂/千克润滑油组合物。当使用两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物时,这些范围是指由该混合物提供的水杨酸皂的量。
术语“水杨酸皂”是指由所述一种或多种碱金属或碱土金属水杨酸盐清净剂贡献的碱金属或碱土金属水杨酸盐的量,不包括任何高碱性材料。
碱金属或碱土金属水杨酸盐(水杨酸皂)的摩尔数可通过使用滴定法,包括两相滴定法,如使用ASTM D664测定的总酸值(TAN)、渗析和其它众所周知的分析技术推导。必须测定金属总量并使用金属比分配在水杨酸和无机酸之间。方便地通过电感耦合等离子体原子发射光谱法-ASTM D4951测定存在的金属总量。金属比被定义为存在的金属总量除以超过中和存在的任何水杨酸所需的量的金属量(即中和无机酸的金属量)。金属比由商业清净剂的制造商给出并可由了解存在的盐总量和水杨酸的平均分子量的制造商测定。可通过渗析清净剂并量化残留物的量来测定清净剂中存在的碱金属或碱土金属水杨酸盐的量。如果不知道水杨酸盐的平均分子量,可用强酸处理来自渗析清净剂的残留物以将盐转化成其酸形式,通过色谱法、质子NMR和质谱法分析并与已知性质的水杨酸相关联。更特别地,渗析清净剂,然后用强酸处理残留物以将任何盐转化成它们各自的酸形式。然后可通过ASTM D1957中描述的方法测量该混合物的羟基值(hydroxide number)。由于水杨酸包括羟基官能团,必须进行单独分析以量化这些羟基的量,从而可校正通过ASTM D1957测定的羟基值。
或者,用于推导碱金属或碱土金属水杨酸盐(水杨酸皂)的摩尔数的第二种方法假定了制造清净剂而装载的所有水杨酸实际上转化成盐。这两种方法都能测定清净剂中存在的水杨酸皂的量。
水杨酸通常通过苯氧化物的羧化,例如通过Kolbe-Schmitt法制备。将水杨酸高碱化的方法是本领域技术人员已知的。
清净剂通常包含极性头和长疏水尾,极性头包含酸性有机化合物的金属盐。该盐可含有基本化学计算量的金属,此时它们通常被描述为正盐或中性盐并通常具有0至80的在100%活性质量下的总碱值或TBN(可通过ASTM D2896测得)。可通过过量金属化合物(如氧化物或氢氧化物)与酸性气体(如二氧化碳)的反应引入大量金属碱。所得高碱性清净剂包含中和的清净剂作为金属碱(例如碳酸盐)胶束的外层。此类高碱性清净剂可具有100或更高,通常200至500或更高的在100%活性质量下的TBN。
合适地,所述一种或多种碱金属或碱土金属水杨酸盐清净剂可以是中性或高碱性的。所述一种或多种碱金属或碱土金属水杨酸盐清净剂具有0至500mg KOH/g的在100%活性质量下的TBN(可通过ASTM D2896测得)。优选地,所述一种或多种碱金属或碱土金属水杨酸盐清净剂是高碱性碱金属或碱土金属水杨酸盐清净剂。优选地,所述一种或多种高碱性碱金属或碱土金属水杨酸盐清净剂具有50至500mg KOH/g,优选100至500mg KOH/g,更优选150至500mg KOH/g,再更优选200至500mg KOH/g,例如250至500mg KOH/g的在100%活性质量下的TBN(可通过ASTM D2896测得)。
优选地,油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物是一种或多种碱金属或碱土金属C8至C30烷基水杨酸盐清净剂,更优选一种或多种碱金属或碱土金属C10至C20烷基水杨酸盐清净剂,最优选一种或多种碱金属或碱土金属C14至C18烷基水杨酸盐清净剂。烷基可以是直链或支化的,且合适的烷基的实例包括:辛基;壬基;癸基;十二烷基;十五烷基;十八烷基;二十烷基;二十二烷基;二十三烷基;二十六烷基;和三十烷基。如本文中定义的水杨酸盐清净剂还可包括其硫化衍生物。
优选地,所述一种或多种碱金属或碱土金属水杨酸盐清净剂是一种或多种碱土金属水杨酸盐清净剂。水杨酸钙和水杨酸镁清净剂特别优选,尤其是水杨酸钙清净剂。
优选地,油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物为润滑油组合物提供基于润滑油组合物的总质量计大于或等于0.3,更优选大于或等于0.4,更优选大于或等于0.5质量%的金属,通过ASTM D5185测得。优选地,油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物为润滑油组合物提供基于润滑油组合物的总质量计小于或等于1.5,更优选小于或等于1.3,再更优选小于或等于1.2质量%的金属,通过ASTM D5185测得。
在润滑油组合物中可存在其它含金属清净剂并包括金属的油溶性中性和高碱性磺酸盐、酚盐、硫化酚盐、硫代膦酸盐和环烷酸盐,特别是碱金属或碱土金属,例如钠、钾、锂、钙和镁的所述盐。最常用的金属是钙和镁(两者都可存在于润滑剂中使用的清净剂中),以及钙和/或镁与钠的混合物。清净剂可以各种组合使用。
在一个优选实施方案中,油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物代表润滑油组合物中仅有的含金属清净剂。
润滑油组合物包含(c)一种或多种油溶性或油分散性无灰分散剂。可用于本发明的无灰分散剂合适地包含具有能与要分散的粒子结合的官能团的油溶性聚合物长链主链。通常,这样的分散剂具有常经由桥连基连接到聚合物主链上的胺、胺-醇或酰胺极性部分。合适的无灰分散剂可以例如选自长链烃取代的单-和多元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;具有直接附着于其上的聚胺部分的长链脂族烃;和通过长链取代酚与甲醛和多亚烷基多胺的缩合形成的曼尼希缩合产物。
适用于本发明中所用的润滑油组合物的分散剂可优选衍生自聚烯基取代的单-或二元羧酸、酐或酯,分散剂具有数均分子量为至少900的聚烯基结构部分和每个聚烯基结构部分多于1.3至1.7,优选多于1.3至1.6,最优选多于1.3至1.5个官能团(单-或二元羧酸生成部分)(中等官能度分散剂)。官能度(F)可根据以下公式测定:
F=(SAP x Mn)/((112,200 x A.I.)-(SAP x MW)) (1)
其中SAP是皂化值(即根据ASTM D94测定的完全中和1克反应产物中的酸基团所消耗的KOH毫克数);Mn是原料烯烃聚合物的数均分子量;A.I.是反应产物的活性成分百分比(其余部分是未反应的烯烃聚合物、羧酸、酐或酯和稀释剂);且MW是羧酸、酐或酯的分子量(例如琥珀酸酐为98)。
通常,各单-或二元羧酸生成部分会与亲核基团(胺、醇、酰胺或酯极性结构部分)反应,且聚烯基取代的羧酸酰化剂中的官能团数决定最终分散剂中的亲核基团数。
分散剂的聚烯基结构部分优选具有至少450,合适地至少700,优选至少900,如450至3000,优选700至3000,更优选900至2400的数均分子量。分散剂的分子量通常表示为聚烯基结构部分的分子量,因为分散剂的确切分子量范围取决于许多参数,包括用于衍生分散剂的聚合物的类型、官能团数和所用亲核基团的类型。
聚合物分子量,尤其是可通过各种已知技术测定。一种方便的方法是凝胶渗透色谱法(GPC),其另外提供分子量分布信息(参见W.W.Yau、J.J.Kirkland和D.D.Bly,″Modern Size Exclusion Liquid Chromatography″,John Wiley and Sons,New York,1979)。另一可用于测定分子量的方法,特别是对较低分子量聚合物而言,是蒸气压渗透法(参见例如ASTM D3592)。
适用于形成在本发明中可用的润滑油组合物中可用的分散剂的聚烯基结构部分优选具有窄分子量分布(MWD),也称为多分散性,由重均分子量(Mw)与数均分子量(Mn)的比率确定。Mw/Mn小于2.2,优选小于2.0的聚合物最合意。合适的聚合物具有1.5至2.1,优选1.6至1.8的多分散性。
用于形成分散剂的合适的烃或聚合物包括均聚物、互聚物或较低分子量烃。一类这样的聚合物包括乙烯和/或至少一种式H2C=CHR1的C3至C28α-烯烃的聚合物,其中R1是包含1至26个碳原子的直链或支化烷基,且其中聚合物含有碳-碳不饱和,优选高度末端亚乙烯基不饱和。此类聚合物优选包含乙烯和至少一种上式的α-烯烃的互聚物,其中R1是具有1至18个碳原子的烷基,更优选是具有1至8个碳原子,再更优选1至2个碳原子的烷基。
另一类可用的聚合物是通过异丁烯、苯乙烯等的阳离子聚合制成的聚合物。这一类型中的常见聚合物包括通过具有35至75质量%的丁烯含量和30至60质量%的异丁烯含量的C4炼油厂料流在路易斯酸催化剂(如三氯化铝或三氟化硼)存在下的聚合获得的聚异丁烯。用于制造聚正丁烯的单体的优选来源是石油进料流,如残液II(Raffinate II)。在本领域中,如在美国专利No.4,952,739中公开了这些原料。聚异丁烯是本发明的最优选主链,因为其容易由丁烯料流通过阳离子聚合(例如使用AlCl3或BF3催化剂)获得。此类聚异丁烯通常含有沿链安置的每聚合物链一个烯属双键的量的残留不饱和。一个优选实施方案利用由纯异丁烯料流或残液I(Raffinate I)料流制成的聚异丁烯制备具有末端亚乙烯基烯烃的反应性异丁烯聚合物。优选地,被称为高反应性聚异丁烯(HR-PIB)的这些聚合物具有至少65%,例如70%,更优选至少80%,最优选至少85%的末端亚乙烯基含量。例如在美国专利No.4,152,499中描述了此类聚合物的制备。HR-PIB是已知的且HR-PIB可以商品名GlissopalTM(来自BASF)和UltravisTM(来自BP-Amoco)购得。
可用的聚异丁烯聚合物通常基于450至3000的烃链。制造聚异丁烯的方法是已知的。聚异丁烯可如下所述通过卤化(例如氯化)、热“烯”反应或通过使用催化剂(例如过氧化物)的自由基接枝官能化。
烃或聚合物主链可使用上文提到的三种方法的任一种或其任何顺序的组合,选择性地在聚合物或烃链上的碳-碳不饱和位点处或沿链无规地官能化,例如用羧酸生成部分(优选酸或酐部分)官能化。
用于使聚合物烃与不饱和羧酸、酐或酯反应和由这些化合物制备衍生物的方法公开在美国专利Nos.3,087,936;3,172,892;3,215,707;3,231,587;3,272,746;3,275,554;3,381,022;3,442,808;3,565,804;3,912,764;4,110,349;4,234,435;5,777,025;5,891,953;以及EP 0 382 450B1;CA-1,335,895和GB-A-1,440,219中。聚合物或烃可通过使用卤素辅助的官能化(例如氯化)法或热“烯”反应在导致官能结构部分或试剂(即酸、酐、酯部分等)主要在碳-碳不饱和(也称为烯键或烯属不饱和)位点处加成到聚合物或烃链上的条件下使聚合物或烃反应而官能化,例如用羧酸生成部分(优选酸或酐)官能化。
选择性官能化可以通过卤化来实现,例如在60至250℃,优选110至160℃,例如120至140℃的温度下使氯或溴经过聚合物0.5至10小时,优选1至7小时而将不饱和α-烯烃聚合物氯化或溴化到基于聚合物或烃的重量计1至8质量%,优选3至7质量%氯或溴。该卤化聚合物或烃(下文称为主链)随后与足量的能将所需数量的官能结构部分加成到主链上的单不饱和反应物,例如单不饱和羧酸反应物在100至250℃,通常180℃至235℃下反应0.5至10小时,例如3至8小时,以使所得产物含有所需摩尔数的单不饱和羧酸反应物/摩尔卤化主链。或者,将主链和单不饱和羧酸反应物混合并在向热材料中加入氯气的同时加热。
可通过经各种方法沿聚合物链无规连接官能结构部分来将烃或聚合物主链官能化。例如,聚合物可以以溶液或固体形式在自由基引发剂存在下用如上所述的单不饱和羧酸反应物接枝。当在溶液中进行时,接枝在100至260℃,优选120至240℃的高温下进行。自由基引发的接枝优选在含有例如基于初始总油溶液计1至50质量%,优选5至30质量%聚合物的矿物润滑油溶液中实现。
可用于将主链官能化的单不饱和反应物包含单-和二元羧酸材料,即酸、酐或酸酯材料,包括(i)单不饱和的C4至C10二元羧酸,其中(a)羧基是邻位的(即位于相邻碳原子上)和(b)所述相邻碳原子的至少一个,优选两者都是单不饱和的一部分;(ii)(i)的衍生物,如(i)的酐或(i)的C1至C5醇衍生的单酯或二酯;(iii)单不饱和的C3至C10单羧酸,其中碳-碳双键与羧基共轭,即具有结构-C=C-CO-;和(iv)(iii)的衍生物,如(iii)的C1至C5醇衍生的单酯或二酯。也可使用单不饱和的羧酸材料(i)-(iv)的混合物。在与主链反应时,单不饱和羧酸反应物的单不饱和变饱和。因此,例如,马来酸酐变成主链取代的琥珀酸酐,丙烯酸变成主链取代的丙酸。此类单不饱和羧酸反应物的实例是富马酸、衣康酸、马来酸、马来酸酐、氯马来酸、氯马来酸酐、丙烯酸、甲基丙烯酸、巴豆酸、肉桂酸和前述这些的低碳烷基(例如C1至C4烷基)酸酯,例如马来酸甲酯、富马酸乙酯和富马酸甲酯。
为了提供所需官能度,单不饱和羧酸反应物,优选马来酸酐通常以基于聚合物或烃的摩尔计等摩尔量至100质量%过量,优选5至50质量%过量的量使用。如果需要,可以通过例如汽提(通常在真空下)从最终分散剂产物中除去未反应的过量单不饱和羧酸反应物。
官能化的油溶性聚合物烃主链然后用亲核反应物,如胺、氨基-醇、醇、金属化合物或其混合物衍生化以形成相应的衍生物。可用于使官能化聚合物衍生化的胺化合物包含至少一种胺,并可包含一种或多种附加胺或其它反应性或极性基团。这些胺可以是烃基胺或可以主要是烃基胺,其中烃基包括其它基团,例如羟基、烷氧基、酰胺基团、腈、咪唑啉基团等。特别可用的胺化合物包括具有每分子1至12,如3至12,优选3至9,最优选6至7个氮原子的具有2至60,如2至40(例如3至20)个总碳原子的单胺和多胺,例如聚烯和聚氧化烯多胺。可以有利地使用胺化合物的混合物,如通过二卤化烷(alkylene dihalide)与氨的反应制成的那些。优选的胺是脂族饱和胺,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;多亚乙基胺,如二亚乙基三胺;三亚乙基四胺;四亚乙基五胺;和多亚丙基胺,如1,2-丙二胺;和二-(1,2-亚丙基)三胺。被称为PAM的此类多亚烷基多胺混合物可购得。特别优选的多亚烷基多胺混合物是通过从PAM产物中蒸馏轻馏分而衍生的混合物。所得混合物,被称为“重”PAM或HPAM,也可购得。例如在美国专利Nos.4,938,881;4,927,551;5,230,714;5,241,003;5,565,128;5,756,431;5,792,730;和5,854,186中描述了PAM和/或HPAM的性质和属性。
本发明的方法中的润滑油组合物中所用的分散剂可通过通常如美国专利Nos.3,087,936、3,254,025和5,430,105中教导的常规方式硼化。分散剂的硼化可容易如下实现:通过用硼化合物,如氧化硼、卤化硼、硼酸和硼酸酯以足以提供每摩尔酰化氮组合物0.1至20原子比例硼的量处理含酰基氮的分散剂。
作为脱水硼酸聚合物(主要是(HBO2)3)出现在产物中的硼被认为以胺盐,例如二酰亚胺的偏硼酸盐的形式连接到分散剂酰亚胺和二酰亚胺上。可以通过将足量硼化合物,优选硼酸通常以浆料形式添加到酰基氮化合物中并在搅拌下在135℃至190℃,例如140℃至170℃下加热1至5小时、接着氮气汽提而进行硼化。或者,可以通过将硼酸添加到二元羧酸材料和胺的热反应混合物中、同时除去水而进行硼处理。也可使用本领域中已知的其它后反应方法。
如果硼化分散剂存在于润滑油组合物中,由该硼化分散剂为润滑油组合物提供的硼量合适地为基于润滑油组合物的总质量计至少10,如至少30,例如至少50或甚至至少65ppm硼。如果存在,硼化无灰分散剂合适地为润滑油组合物提供基于润滑油组合物的总质量计不超过1000,优选不超过750,更优选不超过500ppm硼。
在一个优选实施方案中,所述一种或多种油溶性或油分散性无灰分散剂包含通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺,优选多亚烷基多胺的混合物反应形成的琥珀酰亚胺。聚异丁烯基团的数均分子量合适地为至少450,优选至少700,更优选至少900,如450至3000,优选700至3000,更优选900至2400。在使用多于一种油分散性无灰分散剂的实施方案中,优选各自是通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺,优选多亚烷基多胺的混合物反应形成的琥珀酰亚胺,其中一种分散剂的聚异丁烯基团的数均分子量在900至1500之间且另一种分散剂的聚异丁烯基团的数均分子量在1800至3000之间。在一个特别优选的实施方案中,使用两种油溶性或油分散性无灰分散剂,各自是通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺的混合物反应形成的琥珀酰亚胺,其中一种分散剂的聚异丁烯基团的数均分子量在900至1000之间且另一种分散剂的聚异丁烯基团的数均分子量在2000至2500之间。
优选地,所述一种或多种油溶性或油分散性无灰分散剂以基于组合物质量计0.4至10质量%,优选0.5至8质量%,更优选1至5质量%的量存在于润滑油组合物中。
润滑油组合物可任选进一步包含(d)聚烯取代的琥珀酸酐。这些化合物包括上文关于组分(c)作为官能化的油溶性聚合物烃主链描述的那些(在它们用亲核反应物衍生化之前)。优选的是聚异丁烯取代的琥珀酸酐,其中聚异丁烯基团具有至少450,优选至少700,更优选至少900,如450至3000,优选700至3000,更优选900至2400的数均分子量。优选的化合物(d)是聚异丁烯取代的琥珀酸酐,其中聚异丁烯基团具有900至1000的数均分子量。
在一个优选实施方案中,润滑油组合物进一步包含(d)聚烯取代的琥珀酸酐,优选如上所述的聚异丁烯取代的琥珀酸酐。
当存在时,聚烯取代的琥珀酸酐(d)优选以基于组合物质量计0.1至10质量%,优选0.2至8质量%,更优选0.5至6质量%的量存在于润滑油组合物中。
本发明中使用的润滑油组合物的至少50质量%包含(a)具有润滑粘度的油。这些油在粘度上可在轻质馏分矿物油至重质润滑油的范围内。通常,在100℃下测得的该油的粘度为2至40,如3至15mm2/sec,并具有80至100,如90至95的粘度指数。
天然油包括动物油和植物油(例如蓖麻油、猪油);液体石油和加氢精制的、溶剂处理的或酸处理的链烷型、环烷型和混合链烷-环烷型矿物油。衍生自煤或页岩的具有润滑粘度的油也充当可用的基础油。
合成润滑油包括烃油和卤代烃油,如聚合和互聚烯烃(例如聚丁烯、聚丙烯、丙烯-异丁烯共聚物、氯化聚丁烯、聚(1-己烯)、聚(1-辛烯)、聚(1-癸烯));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);聚苯基(例如联苯、三联苯、烷基化聚酚);和烷基化二苯醚和烷基化二苯硫醚以及它们的衍生物、类似物和同系物。
环氧烷聚合物和互聚物及其末端羟基已通过酯化、醚化等改性的衍生物构成另一类已知的合成润滑油。这些例如为通过环氧乙烷或环氧丙烷的聚合制成的聚氧化烯聚合物、以及聚氧化烯聚合物的烷基和芳基醚(例如分子量为1000的甲基聚异丙二醇醚或分子量为1000至1500的聚乙二醇二苯醚);和它们的单-和多羧酸酯,例如四乙二醇的乙酸酯、混合C3-C8脂肪酸酯和C13氧代酸二酯。
另一类合适的合成润滑油包含二元羧酸(例如邻苯二甲酸、琥珀酸、烷基琥珀酸和链烯基琥珀酸、马来酸、壬二酸、辛二酸、癸二酸、富马酸、己二酸、亚油酸二聚物、丙二酸、烷基丙二酸、链烯基丙二酸)与各种醇(例如丁基醇、己基醇、十二烷基醇、2-乙基己基醇、乙二醇、二乙二醇单醚、丙二醇)的酯。此类酯的具体实例包括己二酸二丁酯、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、亚油酸二聚物的2-乙基己基二酯、和通过1摩尔癸二酸与2摩尔四乙二醇和2摩尔2-乙基己酸反应形成的复合酯。
可用作合成油的酯还包括由C5至C12单羧酸和多元醇和多元醇酯(如新戊二醇、三羟甲基丙烷、季戊四醇、二季戊四醇和三季戊四醇)制成的那些。
硅基油,如聚烷基-、聚芳基-、聚烷氧基-或聚芳氧基硅酮油和硅酸酯油构成合成润滑剂的另一可用类型;此类油包括硅酸四乙酯、硅酸四异丙酯、硅酸四(2-乙基己基)酯、硅酸四(4-甲基-2-乙基己基)酯、硅酸四(对叔丁基苯基)酯、六(4-甲基-2-乙基己基)二硅氧烷、聚(甲基)硅氧烷和聚(甲基苯基)硅氧烷。其它合成润滑油包括含磷的酸的液体酯(例如磷酸三甲苯酯、磷酸三辛酯、癸基膦酸二乙酯)和聚合四氢呋喃。
在本发明的润滑剂中可使用未精制、精制和再精制的油。未精制油是直接获自天然或合成来源的未经进一步提纯处理的那些。例如,直接获自干馏操作的页岩油;直接获自蒸馏的石油;或直接获自酯化且不经进一步处理即使用的酯油是未精制油。
The American Petroleum Institute(API)出版物“Engine Oil Licensing andCertification System”,Industry Services Department,第十四版,1996年12月,附录1,1998年12月将基础油料如下分类:
a)使用表E-1中规定的试验方法,第I类基础油料含有少于90%饱和物和/或多于0.03%硫并具有大于或等于80且小于120的粘度指数。
b)使用表E-1中规定的试验方法,第II类基础油料含有大于或等于90%饱和物和小于或等于0.03%硫并具有大于或等于80且小于120的粘度指数。
c)使用表E-1中规定的试验方法,第III类基础油料含有大于或等于90%饱和物和小于或等于0.03%硫并具有大于或等于120的粘度指数。
d)第IV类基础油料是聚α烯烃(PAO)。
e)第V类基础油料包括未包含在第I、II、III或IV类中的所有其它基础油料。
将基础油料的分析方法制成下表:
表E-1
性质 | 试验方法 |
饱和物 | ASTM D 2007 |
粘度指数 | ASTM D 2270 |
硫 | ASTM D 2622 |
ASTM D 4294 | |
ASTM D 4927 | |
ASTM D 3120 |
本发明优选包括含有大于或等于90%饱和物和小于或等于0.03%硫的那些上述油作为具有润滑粘度的油,例如第II、III、IV或V类。它们还包括衍生自通过费托法合成的烃的基础油料。在费托法中,首先生成含有一氧化碳和氢气的合成气体(或“合成气”),然后使用费托催化剂转化成烃。这些烃通常需要进一步加工才可用作基础油。例如,它们可通过本领域中已知的方法加氢异构化;加氢裂化和加氢异构化;脱蜡;或加氢异构化和脱蜡。合成气可以例如由气体(如天然气或其它气态烃)通过蒸汽重整制成,此时基础油料可被称为气制液(“GTL”)基础油;或由生物质的气化制成,此时基础油料可被称为生物质制油(“BTL”或“BMTL”)基础油;或由煤的气化制成,此时基础油料可被称为煤制液(“CTL”)基础油。但是本发明不限于使用上文提到的基础油料;因此其可例如包括使用第I类基础油料和光亮油。
优选地,本发明中的具有润滑粘度的油含有50质量%或更多的所述基础油料。其可含有60,如70、80或90质量%或更多的所述基础油料或其混合物。具有润滑粘度的油可以基本全部是所述基础油料或其混合物。
优选地,本发明的方法中所用的润滑油组合物包含基于组合物质量计至少60质量%,例如至少70质量%或至少80质量%的具有润滑粘度的油。
在本发明的方法中所用的润滑油组合物中可任选存在其它添加剂。
在一个实施方案中,润滑油组合物进一步包含一种或多种抗磨添加剂。抗磨剂减轻摩擦和过度磨损并通常基于含有硫或磷或两者的化合物,例如能在所涉表面上沉积多硫化物膜的化合物。值得注意的是二烃基二硫代磷酸金属盐,其中金属可以是碱金属或碱土金属,或铝、铅、锡、钼、锰、镍、铜或优选锌。
二烃基二硫代磷酸金属盐可根据已知技术通过如下方式制备:首先形成二烃基二硫代磷酸(DDPA),通常通过一种或多种醇或酚与P2S5反应形成,然后用金属化合物中和所形成的DDPA。例如,可通过使伯醇和仲醇的混合物反应制造二硫代磷酸。或者,可以制备多种二硫代磷酸,其中一种上的烃基在性质上完全是仲烃基,且其它上的烃基在性质上完全是伯烃基。为了制造金属盐,可以使用任何碱性或中性金属化合物,但最常使用氧化物、氢氧化物和碳酸盐。商业添加剂通常由于在中和反应中使用过量碱性金属化合物而含有过量金属。
优选的二烃基二硫代磷酸锌(ZDDP)是二烃基二硫代磷酸的油溶性盐并可由下式表示:
其中R和R’可以是含有1至18,优选2至12个碳原子的相同或不同的烃基,并包括如烷基、烯基、芳基、芳烷基、烷芳基和脂环族基团之类的基团。特别优选作为R和R’基团的是含有2至8个碳原子的烷基。因此,所述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、十二烷基、十八烷基、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。为了获得油溶性,二硫代磷酸中的碳原子(即R和R’)总数通常为大约5或更大。二烃基二硫代磷酸锌因此可包含二烷基二硫代磷酸锌。
ZDDP以足以为润滑油提供基于润滑油组合物的总质量计的按质量计不大于1200ppm,优选不大于1000ppm,更优选不大于900ppm,最优选不大于850ppm磷的量添加到润滑油组合物中,所述量根据ASTM D5185测得。ZDDP合适地以足以为润滑油提供基于润滑油组合物的总质量计的按质量计至少100ppm,优选至少200ppm,例如200至400ppm磷的量添加到润滑油组合物中,所述量根据ASTM D5185测得。
可以使用两种或更多种抗磨添加剂,例如两种或更多种不同的ZDDP化合物的混合物。
下面描述在本发明的方法中所用的润滑油组合物中还可存在的其它添加剂(或共添加剂)。当存在时,共添加剂的量如下文以在润滑油组合物中的活性成分质量%指定。
如本领域中已知,一些添加剂可提供多重作用。
可以使用选自非离子聚氧化烯多元醇及其酯、聚氧化烯酚和阴离子烷基磺酸的防锈剂。
可以使用含铜和铅的缓蚀剂,但其典型地不是本发明的制剂所要求的。此类化合物通常是含有5至50个碳原子的噻二唑多硫化物、它们的衍生物及其聚合物。1,3,4噻二唑的衍生物,如美国专利Nos.2,719,125;2,719,126;和3,087,932中描述的那些是典型的。在美国专利Nos.3,821,236;3,904,537;4,097,387;4,107,059;4,136,043;4,188,299;和4,193,882中描述了其它类似的材料。其它添加剂是噻二唑的硫代和多硫代次磺酰胺,如英国专利说明书No.1,560,830中描述的那些。苯并三唑衍生物也属于这类添加剂。当这些化合物包括在润滑组合物中时,它们优选以不超过0.2重量%活性成分的量存在。
可以使用少量破乳组分。在EP 330522中描述了优选的破乳组分。其通过使环氧烷与由双环氧化物与多元醇反应获得的加合物反应而得。破乳剂应该以不超过0.1质量%活性成分的量使用。0.001至0.05质量%活性成分的处理率是方便的。
可由许多化合物,包括聚硅氧烷型防沫剂,例如硅酮油或聚二甲基硅氧烷提供泡沫控制。
可将各添加剂——必要组分(b)和(c)二者、任选组分(d)和任意共添加剂以任何方便的方式掺入具有润滑粘度的油中。因此,可以通过将其以所需浓度水平分散或溶解在具有润滑粘度的油中而将各组分直接添加到具有润滑粘度的油中。这样的掺合可在环境温度或升高的温度下进行。
优选将所有组分掺合到浓缩物或添加剂包中,随后将浓缩物或添加剂包掺合到具有润滑粘度的油中以制造成品润滑油组合物。通常配制浓缩物以含有适当量的添加剂以在将浓缩物与预定量的具有润滑粘度的油合并时在最终制剂中提供所需浓度。
优选根据US 4,938,880中描述的方法制造浓缩物。该专利描述了制造无灰分散剂和金属清净剂的预混物,其在至少大约100℃的温度下预掺合。此后,将预混物冷却到至少85℃并加入附加组分。
在第二个方面中,本发明提供对第一个方面所限定的润滑油组合物在用符合船用残渣燃料的ISO 8217 2017燃料标准并具有基于燃料质量计大于0.1质量%和小于0.5质量%的硫含量的船用残渣燃料作为燃料的四冲程船用柴油机的运行过程中减少发动机活塞上的沉积物发生率的用途。
下面仅作为实施例描述本发明。
如下表1中所示制备润滑油组合物。所给的量以质量%计,基于油组合物的总质量计。
表1
组分 | 油1 | 油2 | 油3 |
Disp 1 | - | 0.600 | 0.600 |
Disp 2 | - | 2.000 | 2.000 |
Det 1 | 3.755 | 3.755 | 3.755 |
Det 2 | 5.331 | 5.331 | 5.331 |
ZDDP | 0.300 | 0.300 | 0.300 |
PIBSA | - | - | 1.000 |
Gp II油 | 余量 | 余量 | 余量 |
所用组分如下:
Disp 1:硼化(1.3质量%B)无灰分散剂,其是通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺的反应形成的琥珀酰亚胺,聚异丁烯基团具有950的数均分子量。
Disp 2:未硼化的无灰分散剂,其是通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺的反应形成的琥珀酰亚胺,聚异丁烯基团具有2225的数均分子量。
Det 1:水杨酸钙清净剂,其具有通过ASTM D2896测得的350mg KOH/g的TBN和12.5质量%的钙含量。
Det 2:水杨酸钙清净剂,其具有通过ASTM D2896测得的225mg KOH/g的TBN和8质量%的钙含量。
ZDDP:二烷基二硫代磷酸锌,其中60%的烷基是伯C4基团且40%是伯C5基团,且锌含量为8.8质量%。
PIBSA:聚异丁烯取代的琥珀酸酐,其中聚异丁烯基团具有950的数均分子量。
Gp II油:API第II类矿物油
使用聚焦光束反射法(FBRM)评估润滑油组合物的沥青质分散力。这一技术提供沥青质附聚的测量,因此指示润滑油在用于润滑发动机时形成活塞沉积物的趋势。
FBRM试验方法采用光纤探针。探针尖端含有将激光聚焦到小点的光学器件。旋转光学器件以使聚焦光束在窗口上扫描圆形路径,待测量的油样品流过所述窗口。当油中的沥青质粒子流过窗口时,它们与扫描的光路相交,收集由粒子反向散射的光。扫描激光束的行进比粒子快得多,这意味着相对于光,粒子效果上是固定的(effectively stationary)。当聚焦光束与粒子的一条边相交时,收集的反向散射光的量增加,当光束到达粒子的另一边时再次减少。仪器测定检测到增加的反向散射光的时期。将这一时期乘以激光的扫描速度以提供距离。这一距离是弦长,因为其是粒子边缘上的两个点之间的直线的长度。FBRM技术每秒测量数以万计的弦长,因此提供弦长分布,通常以微米表示。由此获得样品中的沥青质粒子的粒度分布的精确测量。
所用FBRM设备是Mettler Toledo,Leicester,UK供应的型号Lasentec G400。其配置为提供1μm至1mm的粒度分辨率。所得数据可以几种方式呈现,但我们的研究表明,每秒平均计数可用作沥青质分散力的定量量度。这一值随平均粒度和附聚度而变。
使用五种不同的船用残渣燃料。这些详列在下表2中。
表2
硫含量(质量%) | 沥青质含量(质量%) | |
燃料1 | 1.9 | 32.11 |
燃料2 | 2.5 | 24.70 |
燃料3 | 1.2 | 12.75 |
燃料4 | 0.47 | 15.25 |
燃料5 | 0.47 | 21.76 |
燃料1–3是符合此类燃料的当前法规(因为它们具有低于3.5质量%的硫含量)并符合船用残渣燃料的ISO 8217 2017燃料标准的船用残渣燃料的实例。这些燃料在2020年1月1日后不能使用,除非使用它们的船舶装有适当的排气净化系统。
燃料4和5是能在2020年1月1日后使用的船用残渣燃料的实例,因为它们具有低于0.5质量%的硫含量。它们也符合船用残渣燃料的ISO 82172017燃料标准的要求。
值得注意的是,较高硫含量燃料和低硫含量燃料都具有明显和类似的沥青质含量。通过ASTM D2007-11的附录X1中给出的“戊烷不溶物”方法测定沥青质含量。
作为第一步骤,通过在多颈平底烧瓶中在搅拌下加热到140℃并经过烧结玻璃管使空气以45升/小时的流量经过该油48小时,人工老化表1中详述的各润滑油组合物的各样品(880g)。
然后将如上所述老化的润滑油组合物的各样品(各49.5g)加热到60℃并在搅拌的同时保持在该温度下。将表2中所列的各燃料的称重样品(9.90g)添加到各油样品中。将FBRM探针插入各混合物中并收集测量结果15分钟。以每秒平均计数表示的所得结果详列在下表3中。各数据点是对各样品的两次单独测量结果的平均值。
表3
燃料1 | 燃料2 | 燃料3 | 燃料4 | 燃料5 | |
油1 | 18126 | 31370 | 1324 | 101.4 | 48280 |
油2 | 34282 | 47583 | 2899 | 61.6 | 10854 |
油3 | 31341 | 41651 | 1750 | 50.4 | 3801 |
对于具有高硫含量的燃料(燃料1-3),表现出独特的行为模式。比较油1和油2的结果,清楚的是,分散剂的添加极大降低该油分散沥青质的能力,以记录的每秒平均计数的大幅提高为证据。在进一步加入PIBSA时看出一些改进(比较油2和3),但油3的性能在每种情况下仍明显不如油1。
对于具有低硫含量的燃料(燃料4和5),看出同样独特但相反的趋势。这里,分散剂的添加(比较油1和油2)使得该油分散沥青质的能力显著提高,通过加入PIBSA进一步改进该行为(比较油2和3)。
这些数据表明本发明的方法能够减少用符合即将生效的IMO 2020法规的残渣燃料运行四冲程船用柴油机中的活塞沉积物的发生率。
使用Ricardo Atlas II四冲程单缸中速发动机评估如上表1中所述的油1、2和3的清洁性能。各自持续60小时,在下列条件下以发动机满负荷和最大额定速度运行:
表4
特征 | |
缸径 | 159mm |
冲程 | 159mm |
功率@额定速度 | 71kW@1500rpm |
转矩@速度 | 452Nm@1500rpm |
BMEP | 18巴 |
汽缸压力 | 160巴 |
这一试验提供润滑剂防止沉积的能力的测量。符合RMG380规范的商业极低硫重质燃料油(VLSFO)用于这些试验(燃料6)。其具有低于0.5质量%的硫含量并符合船用残渣燃料的ISO 8217 2017燃料标准的要求。
表5
硫含量(质量%) | 沥青质含量(质量%) | |
燃料6 | 0.49 | 15.65 |
在试验完成后,(通过DIN 51349-3)视觉评定活塞-环组件的上部区域的在运行过程中形成的沉积物。结果列在表6中。
表6
比较油1与油2和油3的结果,清楚的是,分散剂的添加减少了使用具有低于0.5质量%的硫含量并符合船用残渣燃料的ISO 8217 2017燃料标准的要求的船用残渣燃料运行的发动机中的沉积量。
Claims (22)
1.一种在以符合船用残渣燃料的ISO 8217 2017燃料标准并具有基于燃料质量计大于0.1质量%和小于0.5质量%的硫含量的船用残渣燃料作为燃料的四冲程船用柴油机的运行过程中减少发动机活塞上的沉积物发生率的方法,所述方法包括使用一种润滑油组合物润滑发动机,所述润滑油组合物包含:
(a)基于组合物质量计至少50质量%的具有润滑粘度的油;
(b)基于组合物质量计5至25质量%的油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物,各油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂具有通过ASTM D2896测得的150至500mg KOH/g的总碱值(TBN);和
(c)基于组合物质量计0.5至8质量%的一种或多种油溶性或油分散性无灰分散剂;和任选地,
(d)基于组合物质量计0.1至10质量%的聚烯取代的琥珀酸酐。
2.根据权利要求1的方法,其中所述船用残渣燃料包含选自下组的一种残渣炼油厂料流或两种或更多种的混合物:常压塔底油、真空塔底油、轻循环油、重循环油、流体催化裂化循环油、流体催化裂化油浆、热裂化渣油、热焦油、未稀释焦油、热裂化重质馏分油、I类疏松蜡、脱沥青油、热裂化煤油气制液蜡、加氢精制的轻循环油、加氢精制的重循环油、加氢精制的流体催化裂化循环油、加氢精制的热裂化重质馏分油、加氢精制的塔底油、加氢裂化器蜡乳液和加氢精制的加氢裂化器脱沥青油。
3.根据权利要求1的方法,其中所述船用残渣燃料由选自下组的一种残渣炼油厂料流或两种或更多种的混合物组成:常压塔底油、真空塔底油、轻循环油、重循环油、流体催化裂化循环油、流体催化裂化油浆、热裂化渣油、热焦油、未稀释焦油、热裂化重质馏分油、I类疏松蜡、脱沥青油、热裂化煤油气制液蜡、加氢精制的轻循环油、加氢精制的重循环油、加氢精制的流体催化裂化循环油、加氢精制的热裂化重质馏分油、加氢精制的塔底油、加氢裂化器蜡乳液和加氢精制的加氢裂化器脱沥青油。
4.根据权利要求1的方法,其中所述碱金属或碱土金属是钙,且其中所述油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂代表润滑油组合物中仅有的含金属清净剂。
5.根据权利要求2的方法,其中所述碱金属或碱土金属是钙,且其中所述油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂代表润滑油组合物中仅有的含金属清净剂。
6.根据权利要求3的方法,其中所述碱金属或碱土金属是钙,且其中所述油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂代表润滑油组合物中仅有的含金属清净剂。
7.根据权利要求1-6中任一项的方法,其中所述油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物以基于组合物的总质量计6至20质量%的量存在。
8.根据权利要求7的方法,其中所述油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂、或两种或更多种油溶性或油分散性碱金属或碱土金属水杨酸盐清净剂的混合物以基于组合物的总质量计7至15质量%的量存在。
9.根据权利要求1-6和8中任一项的方法,其中所述一种或多种油溶性或油分散性无灰分散剂包含通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺的反应形成的琥珀酰亚胺。
10.根据权利要求7的方法,其中所述一种或多种油溶性或油分散性无灰分散剂包含通过聚异丁烯取代的琥珀酸酐与多亚烷基多胺的反应形成的琥珀酰亚胺。
11.根据权利要求1-6、8和10中任一项的方法,其中所述润滑油组合物进一步包含(d)聚异丁烯取代的琥珀酸酐。
12.根据权利要求7的方法,其中所述润滑油组合物进一步包含(d)聚异丁烯取代的琥珀酸酐。
13.根据权利要求9的方法,其中所述润滑油组合物进一步包含(d)聚异丁烯取代的琥珀酸酐。
14.根据权利要求11的方法,其中所述聚异丁烯取代的琥珀酸酐的量为0.2至8质量%。
15.根据权利要求12的方法,其中所述聚异丁烯取代的琥珀酸酐的量为0.2至8质量%。
16.根据权利要求13的方法,其中所述聚异丁烯取代的琥珀酸酐的量为0.2至8质量%。
17.根据权利要求14-16中任一项的方法,其中所述聚异丁烯取代的琥珀酸酐的量为0.5至6质量%。
18.根据权利要求1-6、8、10和12-16中任一项的方法,其中所述润滑油组合物进一步包含一种或多种抗磨添加剂。
19.根据权利要求18的方法,其中所述一种或多种抗磨添加剂包含二烃基二硫代磷酸锌盐。
20.根据权利要求1-6、8、10、12-16和19中任一项的方法,其中所述一种或多种油溶性或油分散性无灰分散剂的量为1至5质量%。
21.根据权利要求17的方法,其中所述一种或多种油溶性或油分散性无灰分散剂的量为1至5质量%。
22.根据权利要求1-6、8、10、12-16、19和21中任一项的方法,其中润滑油组合物包含基于润滑油组合物的质量30至500ppm的硼。
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