JP2005320441A - Ultra-low sulfur content engine oil - Google Patents
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本発明は、硫黄分が少なく、耐摩耗性に優れた超低硫黄分エンジン油に関する。 The present invention relates to an ultra-low sulfur engine oil having a low sulfur content and excellent wear resistance.
近年、エンジンには排出ガスの低減が強く求められている。今後更なる排出ガス低減を達成するにはエンジン自体の排出ガスの低減はもとより、後処理装置を加えた全体システムによる低減が必要となってくる。NOxを低減する後処理手段としてNOx低減触媒が検討されているが、本触媒は排出ガス中の硫黄分の影響により性能が劣化する。すなわち燃料及びエンジン油に含有している硫黄分がNOx低減触媒の性能を劣化させ長期間の使用が困難となる。排出ガスの一部となるエンジン油の油消費量は、燃料消費量の１/１０００程度と言われており、現状の平均的な硫黄含有量である０.５質量％の硫黄分を有するエンジン油を用いた場合、仮に燃料中の硫黄分を０としても、燃料中に硫黄分が５質量ppm存在しているのと同じ影響を触媒に与える。 In recent years, there has been a strong demand for engines to reduce exhaust emissions. In order to achieve further emission reductions in the future, it will be necessary to reduce not only the emissions of the engine itself, but also the overall system with an aftertreatment device. A NOx reduction catalyst has been studied as a post-treatment means for reducing NOx, but the performance of this catalyst deteriorates due to the influence of sulfur in the exhaust gas. That is, the sulfur content contained in the fuel and engine oil deteriorates the performance of the NOx reduction catalyst, making it difficult to use for a long time. The oil consumption of engine oil, which is part of the exhaust gas, is said to be about 1/1000 of the fuel consumption, and the engine has a sulfur content of 0.5% by mass, which is the current average sulfur content. When oil is used, even if the sulfur content in the fuel is set to 0, the catalyst has the same effect as the presence of 5 ppm by mass of sulfur in the fuel.
エンジン油は基油と添加剤により製造されるが、従来のエンジン油は０.５質量％前後の硫黄分を含有している。これらの硫黄分は、基油及び添加剤それぞれに含有している。特にエンジン油としての必須の添加剤であるジチオリン酸亜鉛（以下ZnDTP）は耐摩耗性の要求から通常リン量で０.１質量％程度添加され、その添加量は硫黄分としては０.２質量％に相当する。一方、ZnDTPを添加しないとエンジン油としての耐摩耗性を十分維持できないという問題が生じる。 Engine oil is produced with a base oil and additives, but conventional engine oil contains a sulfur content of around 0.5% by mass. These sulfur contents are contained in the base oil and the additive, respectively. In particular, zinc dithiophosphate (hereinafter ZnDTP), which is an essential additive for engine oils, is usually added in an amount of about 0.1% by mass of phosphorus due to the requirement of wear resistance. %. On the other hand, unless ZnDTP is added, there arises a problem that sufficient wear resistance as engine oil cannot be maintained.
本発明者は、上記状況に鑑み鋭意研究を進め、特定の基油と添加剤を組み合わせることで、従来のエンジン油の約１/１０である硫黄分５００ppm以下の低硫黄分エンジン油が製造できるか検討を行った。その結果、基油として硫黄分１００ppm以下の鉱油及び又は合成油を用い、添加剤としてアルキルジエタノールアミドとモノグリセリドの混合物を一部ホウ素化した化合物を添加することで耐摩耗性に優れた硫黄分500ppm以下の超低硫黄分エンジン油が得られることを見いだした。
本発明はかかる知見に基づきなされたものであり、本発明の目的は、超低硫黄分で、かつ耐摩耗性に優れたNOx低減触媒に好適なエンジン油を提供することにある。
The present inventor has conducted earnest research in view of the above situation, and can produce a low sulfur content engine oil having a sulfur content of 500 ppm or less, which is about 1/10 of a conventional engine oil, by combining a specific base oil and an additive. I examined. As a result, mineral oil with a sulfur content of 100 ppm or less as the base oil and / or synthetic oil, and a sulfur content of 500 ppm with excellent wear resistance by adding a partially boronated compound of a mixture of alkyldiethanolamide and monoglyceride as an additive The following ultra-low sulfur engine oil was found to be obtained.
The present invention has been made based on such knowledge, and an object of the present invention is to provide an engine oil suitable for a NOx reduction catalyst having an ultra-low sulfur content and excellent wear resistance.
本発明は、基油として硫黄分１００ppm以下の鉱油及び又は合成油を用い、添加剤としてアルキルジエタノールアミドとモノグリセリド、及びそれらをホウ素化したホウ素化物の混合物を含有することを特徴とする硫黄分５００ppm以下の超低硫黄分エンジン油である。
また、前記混合物に含まれるホウ素化物の割合が２質量％以下であることが好ましい。
The present invention uses mineral oil and / or synthetic oil having a sulfur content of 100 ppm or less as a base oil, and contains a mixture of alkyl diethanolamide and monoglyceride as an additive, and a boride obtained by boronizing them, and has a sulfur content of 500 ppm. The following ultra-low sulfur engine oils.
Moreover, it is preferable that the ratio of the boride contained in the said mixture is 2 mass% or less.
本発明の超低硫黄分エンジン油は、従来のエンジン油の約１/１０の硫黄含有量でありながら、耐摩耗性に優れたエンジン油であり、さらにNOx低減触媒が装着されたエンジンの低排出ガス特性を長期間に渡って持続できるという格別の効果を奏する。 The ultra-low sulfur engine oil of the present invention is an engine oil having excellent wear resistance while having a sulfur content of about 1/10 of that of a conventional engine oil, and is further low in an engine equipped with a NOx reduction catalyst. There is a special effect that the exhaust gas characteristics can be maintained for a long time.
本発明における硫黄分１００ppm以下の鉱油系基油は、ワックスの水素異性化或いは重質油の水素化分解で得られた生成油を溶剤脱ロウまたは水素化脱ロウすることにより得ることができる。また、合成油としては、αオレフインのオリゴマー、ジエステル、ポリオールエステル等が使用できる。 The mineral base oil having a sulfur content of 100 ppm or less in the present invention can be obtained by solvent dewaxing or hydrodewaxing the product oil obtained by hydroisomerization of wax or hydrocracking of heavy oil. As synthetic oils, α-olefin oligomers, diesters, polyol esters and the like can be used.
本発明に使用する混合物は、次の化１〜化５にそれぞれ示されるアルキルジエタノールアミド（化１）、モノグリセリド（化２）、それらをホウ素化したホウ素化物（化３：アルキルジエタノールアミドのホウ素化物、化４、化５：モノグリセリドのホウ素化物）の混合物である。
本発明で使用する混合物としては、アルキルジエタノールアミドとモノグリセリド及びそれらのホウ素化物が含まれているものであれば、特に限定するものではない。アルキルジエタノールアミド、モノグリセリド、アルキルジエタノールアミドのホウ素化物、及びモノグリセリドのホウ素化物を適宜の割合で混合したものでも、アルキルジエタノールアミドとモノグリセリドの混合物を一部ホウ素化して得られる、上記化１〜化５の化合物が混在する混合物が好適に使用できる。
前記混合物において、アルキルジエタノールアミドとモノグリセリドの割合、及びアルキルジエタノールアミドのホウ素化物とモノグリセリドのホウ素化物の割合は、特に限定されず、好ましくは５：９５〜９５：５の範囲内で任意の割合で含まれていればよい。
The mixture used in the present invention is not particularly limited as long as it contains alkyl diethanolamide, monoglyceride, and boronated products thereof. Even if what mixed the alkyl diethanolamide, the monoglyceride, the boronated product of the alkyl diethanolamide, and the boronated product of the monoglyceride in an appropriate ratio, it is obtained by partially boronating the mixture of the alkyl diethanolamide and the monoglyceride. A mixture containing the above compound can be preferably used.
In the mixture, the ratio of the alkyl diethanolamide and the monoglyceride, and the ratio of the alkyl diethanolamide borate and the monoglyceride borate are not particularly limited, and preferably in an arbitrary ratio within the range of 5:95 to 95: 5. It only has to be included.
化１〜化５の化合物の混合物中に、ホウ素化物は２質量％以下の割合で含まれていることが好ましい。すなわち、アルキルジエタノールアミドのホウ素化物（化３）とモノグリセリドのホウ素化物（化４、化５）が全く含まれていないと、耐摩耗性は特に改善されないが、前記ホウ素化物が微量でも含まれると、好ましくは、０.１質量％以上含まれると、耐摩耗性は格段に向上する。また、ホウ素化物の割合が２質量％を超えても、耐摩耗性はあまり向上しない。ホウ素化物の割合は、０.５〜２質量％がより好ましい。 It is preferable that the boride is contained in the mixture of the chemical compounds 1 to 5 at a ratio of 2% by mass or less. That is, if the boronic acid alkyl diethanolamide (Chemical Formula 3) and the monoglyceride boronic acid (Chemical Formula 4, Chemical Formula 5) are not included at all, the wear resistance is not particularly improved. Preferably, when it is contained in an amount of 0.1% by mass or more, the wear resistance is remarkably improved. Moreover, even if the ratio of boride exceeds 2 mass%, abrasion resistance does not improve so much. As for the ratio of a boride, 0.5-2 mass% is more preferable.
また、前記混合物は、潤滑油基油に対して０.１〜５質量％、さらには０.５〜２質量％添加することが好ましい。こうすることにより、硫黄含有添加剤の添加量を削減してNOx低減触媒に好適な環境をもたらし、かつ耐摩耗性に優れたエンジン油を提供することができる。 Moreover, it is preferable that the said mixture is 0.1-5 mass% with respect to lubricating base oil, Furthermore, 0.5-2 mass% is added. By doing so, it is possible to provide an engine oil that reduces the amount of the sulfur-containing additive added to provide a suitable environment for the NOx reduction catalyst and is excellent in wear resistance.
さらに、本発明のエンジン油には、エンジン油として通常用いられるコハク酸イミド、コハク酸エステル、ヒドロキシベンジルアミン等の分散剤、フェノール系、アミン系等の酸化防止剤、オレフィンコポリマー、ポリメタクリレート等の粘度指数向上剤及びシリコーン系等の消泡剤、流動点降下剤等を適宜添加できる。 Furthermore, the engine oil of the present invention includes dispersants such as succinimides, succinates, and hydroxybenzylamines that are commonly used as engine oils, phenolic and amine antioxidants, olefin copolymers, polymethacrylates, and the like. Viscosity index improvers, silicone-based antifoaming agents, pour point depressants, and the like can be added as appropriate.
次に、実施例及び比較例により本発明を具体的に説明する。 Next, the present invention will be specifically described with reference to Examples and Comparative Examples.
硫黄分１００ppmの以下の基油は、下記の方法で得た。沸点４００〜５５０℃のスラックワックスをＮｉ-Ｍｏ担持アルミナ触媒の存在下に、水素分圧８０kg/cm2、温度３９０℃、ＬＨＳＶ ０.５Hr-1の反応条件で水添異性化した。得られた異性化油を蒸留し、３５０℃以下の留分を留去して得られた留分を、ＭＥＫ/トルエン混合溶媒を用いて−２０℃で脱蝋して得た。得られた基油の性状を表1に示す。 The following base oil having a sulfur content of 100 ppm was obtained by the following method. Slack wax having a boiling point of 400 to 550 ° C. was hydroisomerized in the presence of a Ni—Mo supported alumina catalyst under the reaction conditions of a hydrogen partial pressure of 80 kg / cm 2 , a temperature of 390 ° C., and LHSV 0.5 Hr −1 . The obtained isomerized oil was distilled and a fraction obtained by distilling a fraction of 350 ° C. or lower was obtained by dewaxing at −20 ° C. using a MEK / toluene mixed solvent. Table 1 shows the properties of the obtained base oil.
表２に示す実施例及び比較例のエンジン油を調整し、各種評価を実施した。アルキルジエタノールアミド、モノグリセリド及びそれらのホウ素化化合物の混合物としては、アルキルジエタノールアミドとモノグリセリドからなる混合物（混合モル比、７０：３０、アルキル基の炭素数は７〜１７の混合）の一部をホウ素化して得た混合物（ホウ素化物として１質量％含有）を、他の添加剤とともに表２に示す割合（重量％）で配合した。 Various engine oils of Examples and Comparative Examples shown in Table 2 were prepared and subjected to various evaluations. As a mixture of alkyldiethanolamide, monoglyceride and boronated compounds thereof, a part of a mixture composed of alkyldiethanolamide and monoglyceride (mixing molar ratio, 70:30, mixture of alkyl group having 7 to 17 carbon atoms) is boron. A mixture (containing 1% by mass as a boride) was blended with other additives in the proportions (% by weight) shown in Table 2.
表２に示すエンジン油について、下記評価を実施し、エンジン油としての性能を確認した。結果を表３に示す。
・耐摩耗性：シェル四球摩耗試験（JPI-5S-32-90）
回転数1200rpm、荷重30kgf、温度80℃、60 min
・動弁系摩耗防止性：4D34T4動弁系摩耗試験（JASO M354）
About the engine oil shown in Table 2, the following evaluation was implemented and the performance as engine oil was confirmed. The results are shown in Table 3.
・ Abrasion resistance: Shell four-ball wear test (JPI-5S-32-90)
Rotation speed 1200rpm, load 30kgf, temperature 80 ℃, 60 min
・ Valve wear resistance: 4D34T4 Valve wear test (JASO M354)
実施例1は、硫黄分が４６０ppmと低く、かつシェル四球摩耗試験での摩耗痕径が0.28mmと小さく、良好な耐摩耗性を有している。さらに、4D34T4動弁系摩耗試験のカム摩耗が３６.６μmとディーゼルエンジン油に関するJASO DH-1規格の合格基準９５μm以下を、余裕をもってクリアしている。 In Example 1, the sulfur content is as low as 460 ppm, the wear scar diameter in the shell four-ball wear test is as small as 0.28 mm, and the wear resistance is good. In addition, the cam wear of the 4D34T4 valve train wear test is 36.6 μm, which satisfies the JASO DH-1 standard of 95 μm or less for diesel engine oil with a margin.
比較例１は、シェル四球試験の摩耗痕径は０.３２mmと耐摩耗性に関してはまずまずであるが、硫黄分が２４００ppmと高く、NOx低減触媒適合性に劣る。 In Comparative Example 1, the wear scar diameter of the shell four-ball test is 0.32 mm, which is reasonable with respect to wear resistance, but the sulfur content is as high as 2400 ppm, which is inferior in NOx reduction catalyst compatibility.
比較例２は、比較例1からZnDTPを除去したものであるが、硫黄分は低減されるがシェル四球試験での摩耗痕径が０.３６mmと耐摩耗性に劣る。 Comparative Example 2 is obtained by removing ZnDTP from Comparative Example 1. Although the sulfur content is reduced, the wear scar diameter in the shell four-ball test is 0.36 mm, which is inferior in wear resistance.
以上の結果から明らかなように、基油として硫黄分１００ppm以下の鉱油又は合成油を用い、アルキルジエタノールアミドとモノグリセリドの一部をホウ素化して得た混合物を添加することで、良好な耐摩耗性を有する、硫黄分５００ppm以下の超低硫黄分エンジン油を得ることができることが確認された。 As is clear from the above results, by using a mineral oil or synthetic oil having a sulfur content of 100 ppm or less as a base oil, and adding a mixture obtained by boronating a part of alkyldiethanolamide and monoglyceride, good abrasion resistance It was confirmed that an ultra-low sulfur engine oil having a sulfur content of 500 ppm or less can be obtained.
以上のような本発明の超低硫黄分エンジン油は、従来のエンジン油の約１/１０の硫黄含有量でありながら、耐摩耗性に優れたエンジン油で、NOx低減触媒が装着されたエンジンの低排出ガス特性を長期間に渡って持続できるという格別の効果を奏する。
The ultra-low sulfur engine oil of the present invention as described above is an engine oil having excellent wear resistance while having a sulfur content of about 1/10 that of a conventional engine oil, and is equipped with a NOx reduction catalyst. It has a special effect that the low exhaust gas characteristics can be maintained for a long time.
Claims (2)
The ultra-low sulfur engine oil according to claim 1, wherein a ratio of boride contained in the mixture is 2% by mass or less.
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| WO2011068137A1 (en) * | 2009-12-03 | 2011-06-09 | 出光興産株式会社 | Lubricating oil composition |
| WO2014070314A1 (en) | 2012-10-30 | 2014-05-08 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
| WO2014070309A1 (en) | 2012-10-30 | 2014-05-08 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
| WO2014070268A2 (en) | 2012-10-30 | 2014-05-08 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
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| JP2009529603A (en) * | 2006-04-26 | 2009-08-20 | アール．ティー． ヴァンダービルト カンパニー インコーポレーティッド | Antioxidant synergist for lubricating compositions |
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| WO2014070309A1 (en) | 2012-10-30 | 2014-05-08 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
| WO2014070268A2 (en) | 2012-10-30 | 2014-05-08 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
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| JP2015533386A (en) * | 2012-10-30 | 2015-11-24 | シェブロン・オロナイト・カンパニー・エルエルシー | Friction modifier and method for producing the same |
| JP2015536369A (en) * | 2012-10-30 | 2015-12-21 | シェブロン・オロナイト・カンパニー・エルエルシー | Friction modifier and method for producing the same |
| US9227920B2 (en) | 2012-10-30 | 2016-01-05 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
| US9371499B2 (en) | 2012-10-30 | 2016-06-21 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
| US9388362B2 (en) | 2012-10-30 | 2016-07-12 | Chevron Oronite Company Llc | Friction modifiers and a method of making the same |
| CN110003969A (en) * | 2012-10-30 | 2019-07-12 | 雪佛龙奥伦耐有限责任公司 | Friction improver and its manufacturing method |
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