TWI490330B - Lubricant oil composition and method for manufacturing the same - Google Patents

Lubricant oil composition and method for manufacturing the same Download PDF

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TWI490330B
TWI490330B TW099146827A TW99146827A TWI490330B TW I490330 B TWI490330 B TW I490330B TW 099146827 A TW099146827 A TW 099146827A TW 99146827 A TW99146827 A TW 99146827A TW I490330 B TWI490330 B TW I490330B
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lubricating oil
nano
oil composition
polymer chain
diamond
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TW099146827A
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TW201226551A (en
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Yu Lin Hsin
Mei Hua Wang
Chih Kuang Chang
ting yao Su
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Ind Tech Res Inst
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潤滑油組合物及其製配方法Lubricating oil composition and preparation method thereof

本發明係關於一種奈米潤滑油組合物及其製配方法,特別關於一種不需添加分散劑或界面活性劑之奈米潤滑油組合物及其製配方法。The present invention relates to a nano lubricating oil composition and a method for preparing the same, and more particularly to a nano lubricating oil composition which does not require the addition of a dispersing agent or a surfactant, and a method for preparing the same.

環境汙染是近年最被關注全球性問題,尤其是二氧化碳排放及臭氧破壞造成溫室效應更是全球暖化元凶。增加機械動力效率不僅節省成本更可以減少能源使用,間接減少二氧化碳的排放。減少機械引擎內磨擦力是主要增加能源效率方式,而潤滑油使用便是減少摩擦力增加效率的必要方法,潤滑油特性也影響整個內燃機或機械組件效率。除了適當的潤滑油特性改良外,添加適合的不同添加劑於潤滑油裡能也是在降低磨擦阻力方式。目前較高級的潤滑油添加劑為有機硫、磷、氯衍生物,雖然具有很好潤滑性,如日本專利8-20786所揭露使用二烷基二硫代甲酸鉬(molybdenum dithiocarbamate,MoDTC)以及二硫代磷酸鉬(molybdenum dithiophosphate,MoDTP),但其最大缺點為不耐高溫、高壓、壽命短、環境汙染。無機固體潤滑油添加劑如石墨、二硫化鉬、奈米鑽石具有高溫高壓穩定性和較高壽命。其中二硫化鉬容易氧化且會造成環境污染,大部分國家已經禁止使用這類的固體添加劑。而石墨常因為顆粒過大無法有效懸浮因而沉澱並阻塞油路。Environmental pollution is the most concerned global issue in recent years, especially the greenhouse effect caused by carbon dioxide emissions and ozone destruction is the global warming. Increasing mechanical power efficiency not only saves costs but also reduces energy use and indirectly reduces carbon dioxide emissions. Reducing the friction in the mechanical engine is a major way to increase energy efficiency, and the use of lubricating oil is a necessary method to reduce the friction to increase efficiency, and the lubricating oil characteristics also affect the efficiency of the entire internal combustion engine or mechanical components. In addition to the appropriate improvement in lubricating oil properties, the addition of suitable different additives to the lubricating oil can also reduce the frictional resistance. At present, higher-grade lubricating oil additives are organic sulfur, phosphorus, and chlorine derivatives. Although they have good lubricity, as disclosed in Japanese Patent No. 8-20786, molybdenum dithiocarbamate (MoDTC) and disulfide are disclosed. Molybdenum dithiophosphate (MoDTP), but its biggest disadvantage is that it is not resistant to high temperature, high pressure, short life and environmental pollution. Inorganic solid lubricating oil additives such as graphite, molybdenum disulfide, and nanodiamonds have high temperature and high pressure stability and high life. Among them, molybdenum disulfide is easily oxidized and causes environmental pollution, and most countries have banned the use of such solid additives. Graphite often precipitates and blocks the oil path because the particles are too large to float effectively.

超分散奈米鑽石(Ultra dispersed diamond,UDD)核心為鑽石結構,而最外層覆蓋石墨層狀結構,是為純碳的材料。奈米鑽石為無環境污染、耐高溫、極佳導熱率、核心具極高硬度和表面具有良好潤滑性。超分散鑽石(Ultra dispersed diamond,UDD)之粒徑約4-6奈米,是以瞬間爆炸法合成,在負氧平衡的條件下炸高溫超高壓環境中爆炸產生游離碳轉變成鑽石顆粒。在此瞬間爆炸產生的環境,並非所有碳源全轉變成鑽石結構,部分游離碳形成類富勒烯(fullerene like)結構碳覆蓋鑽石顆粒,並聚集成直徑數百奈米甚至數微米的顆粒。此種奈米鑽石顆粒約4-6奈米,具有最大硬度、極高導熱性、較高耐磨性、和良好化學穩定性等鑽石的一般特性外。但此種奈米鑽石具有非常高比表面積(280-420m2 /g),奈米鑽石不僅具有極高表面能量還因表面化學鍵結具有強烈團聚傾向,自我團聚成數微米凝結體。這些團聚現象使得奈米鑽石失去奈米特性,這些團聚凝結體的尺寸超過數微米,其磨擦特性、流動性、分散性受到很大影響。The ultra-dispersed nano-diamond (UDD) core is a diamond structure, while the outermost layer covers the graphite layer structure and is a pure carbon material. Nano diamonds are environmentally friendly, resistant to high temperatures, excellent thermal conductivity, high core hardness and good lubricity on the surface. The ultra-dispersed diamond (UDD) has a particle size of about 4-6 nm. It is synthesized by an instantaneous explosion method. Under the condition of negative oxygen balance, the explosion produces a free carbon and turns into a diamond particle in a high-temperature and ultra-high pressure environment. In this instant explosion environment, not all carbon sources are completely converted into diamond structure, and some free carbon forms fullerene like structural carbon covering diamond particles and aggregates into particles of several hundred nanometers or even several micrometers in diameter. Such nanodiamond particles are about 4-6 nm, and have the general properties of diamonds such as maximum hardness, extremely high thermal conductivity, high wear resistance, and good chemical stability. However, such nano-diamonds have a very high specific surface area (280-420 m 2 /g), and nano-diamonds not only have extremely high surface energy but also have a strong agglomeration tendency due to surface chemical bonding, self-aggregating into several micron coagulation bodies. These agglomeration phenomena cause the nano-diamonds to lose their nano-characteristics. These agglomerates have a size exceeding a few micrometers, and their friction characteristics, fluidity, and dispersibility are greatly affected.

為了解決這個問題,中國專利CN02139764.3中揭露將超分散奈米鑽石以高速氣流對撞超細粉末,並加入表面活性劑、分散穩定劑、PH調節劑等以超音波及攪拌方式使其分散於水溶液中。然而該方法為奈米鑽石親水性表面改性,在潤滑油裡無法達到分散效果。同樣類似專利CN02115230.6以超音波方式分散解團聚,並加入不同矽烷表面活性劑,使其能分散於水相或油相中。而在中國專利CN001695779A中更進一步揭露以高速剪切機並利用超音波震盪使超分散奈米鑽石解團聚,加入界面性劑使其分散於潤滑油中。美國發明專利2008248979A1中便公開一種潤滑油添加界面活性劑及奈米鑽石,使奈米鑽石能分散於潤滑油中並有效降低磨擦阻力。雖然以界面活性劑以物理吸附奈米鑽石而分散於潤滑油中,然而過多界面活性劑也將影響整潤滑特性,以物理吸附方式在高溫情況下不穩定。因此該潤滑油因機件運作過程中逐漸升溫,在油溫升高到一定程度下奈米鑽石因界面活性劑脫附再次團聚成較大凝結體,而過大凝結體不僅不具有潤滑特性反而產生刮損情況。In order to solve this problem, Chinese Patent No. CN02139764.3 discloses that ultra-dispersed nano-diamonds are collided with ultra-fine powder by high-speed airflow, and surfactant, dispersion stabilizer, pH adjuster, etc. are added to disperse by ultrasonic wave and stirring method. In an aqueous solution. However, this method is a hydrophilic surface modification of nano diamonds, and the dispersion effect cannot be achieved in the lubricating oil. Similarly, the similar patent CN02115230.6 disperse and agglomerate in an ultrasonic manner, and add different decane surfactants to disperse in the aqueous phase or the oil phase. Further, in Chinese patent CN001695779A, a high-speed shearing machine is used to deagglomerate the super-dispersed nano-diamond by ultrasonic vibration, and an interfacial agent is added to disperse it in the lubricating oil. U.S. Patent No. 2008248979A1 discloses a lubricating oil-adding surfactant and a nano-diamond, which enables the nano-diamond to be dispersed in the lubricating oil and effectively reduce the frictional resistance. Although the surfactant is physically dispersed in the lubricating oil by dispersing the nano-diamond, the excessive surfactant will also affect the overall lubricating property and be unstable under high temperature conditions by physical adsorption. Therefore, the lubricating oil gradually heats up during the operation of the machine. When the oil temperature rises to a certain extent, the nano-diamond reaggregates into a larger coagulation body due to the desorption of the surfactant, and the excessively large coagulated body not only has no lubricating property but instead produces Scratch damage.

奈米鑽石雖具有良好特性,卻因為本身不相容於潤滑油造成團聚現象,雖有以界面活性劑改善其相容問題,但添加界面活性劑之潤滑油在長期機械運作下會因高溫造成表面活性劑脫附,最後仍然造成納米鑽石團聚,其效果和耐久度仍然無法有效令人滿意的。另外添加過多介面活性劑甚至可能和其他潤滑添加劑如清凈劑、腐蝕及銹蝕劑、抗氧化劑等相互產生影響,造成其他添加劑功能喪失或降低。Although nano-diamonds have good characteristics, they are agglomerated due to their incompatibility with lubricating oil. Although surfactants improve compatibility problems, lubricants with surfactants are caused by high temperature during long-term mechanical operation. Surfactant desorption eventually leads to the agglomeration of nanodiamonds, and its effectiveness and durability are still not effectively satisfactory. In addition, adding too much surfactant may even affect other lubricating additives such as detergents, corrosion and rust inhibitors, antioxidants, etc., causing loss or reduction of other additives.

本發明的目的正是基於上述理由,發展一種奈米鑽石為基材的有機/無機複合納米粒子,不僅具有與潤滑油高度相容的外層有機層,且仍具有內層無機層奈米鑽石特性,不須額外添加介面活性劑或分散劑,又能改良其油相分散問題及耐久性問題,是目前奈米鑽石應用於工業用途最需要的技術。The purpose of the present invention is to develop an organic/inorganic composite nanoparticle based on nano-diamonds based on the above reasons, which not only has an outer layer organic layer which is highly compatible with lubricating oil, but also has an inner layer inorganic layer nano-diamond characteristic. It does not require additional addition of surfactants or dispersants, and can improve its oil phase dispersion and durability problems. It is currently the most needed technology for nano diamonds for industrial applications.

本發明提供一種潤滑油組合物及其製備方法。本發明所述之潤滑油組合物由一基礎潤滑油以及一均勻分散於該基礎潤滑油之有機無機奈米複合粒子所組成,可以在不添加任何分散劑或界面活性劑的狀況下,仍達到大幅降低磨耗阻力、油溫和磨耗量的目的。The invention provides a lubricating oil composition and a preparation method thereof. The lubricating oil composition of the present invention comprises a base lubricating oil and an organic-inorganic nano composite particle uniformly dispersed in the base lubricating oil, and can still be achieved without adding any dispersing agent or surfactant. Greatly reduce wear resistance, oil temperature and wear.

本發明提供一種潤滑油組合物,基本上由以下成份所組成:一基礎潤滑油;以及,一均勻分散於該基礎潤滑油之有機/無機奈米複合粒子。The present invention provides a lubricating oil composition consisting essentially of: a base lubricating oil; and an organic/inorganic nanocomposite particle uniformly dispersed in the base lubricating oil.

本發明亦提供一種潤滑油組合物的製備方法,包括:將一奈米鑽石顆粒與一反應單體混合,得到一混合物;對該混合物進行一濕式球磨解團聚製程及一聚合反應,以形成一表面具有接枝高分子鏈的奈米鑽石顆粒;以及,將該表面具有接枝高分子鏈的奈米鑽石顆粒與一基礎潤滑油混合,並進行一分散程序。The invention also provides a method for preparing a lubricating oil composition, comprising: mixing one nanometer diamond particles with a reactive monomer to obtain a mixture; performing a wet ball milling agglomeration process and a polymerization reaction on the mixture to form a nano-diamond particle having a grafted polymer chain on a surface; and a nano-diamond particle having a grafted polymer chain on the surface thereof is mixed with a base lubricating oil, and a dispersion process is performed.

本發明的優點目的在於:克服以往技術缺失,習知添加過多界面活性劑分散奈米鑽石,其耐久性不佳且會影響其他潤滑油添加劑,本發明的潤滑油組合物不需添加任何的分散劑或表面活性劑,即使在長期運作下,該有機/無機奈米複合粒子仍可以穩定分散於該基礎潤滑油中,降低磨耗阻力。因此,本發明的潤滑油組合物可應用于自動車內燃機或動力機械滑動組件上,可大幅降低磨擦力、油溫和機械磨耗率。The invention has the advantages of overcoming the prior art, and it is conventional to add too much surfactant dispersing nano diamond, which has poor durability and affects other lubricating oil additives, and the lubricating oil composition of the invention does not need to be added any dispersion. The organic or inorganic nano composite particles can be stably dispersed in the base lubricating oil even under long-term operation, thereby reducing the abrasion resistance. Therefore, the lubricating oil composition of the present invention can be applied to an internal combustion engine or a power mechanical sliding assembly, and the frictional force, oil temperature, and mechanical wear rate can be greatly reduced.

以下藉由數個實施例並配合所附圖式,以更進一步說明本發明之方法、特徵及優點,但並非用來限制本發明之範圍,本發明之範圍應以所附之申請專利範圍為準。The method, features, and advantages of the present invention are further illustrated by the accompanying drawings, which are set forth in the accompanying drawings. quasi.

本發明提供一種潤滑油組合物,係由一基礎潤滑油以及一均勻分散於該基礎潤滑油之有機無機奈米鑽石奈米複合粒子(organic-inorganic nanodiamond composite particles)所組成。該潤滑油組合物不需添加任何之分散劑或界面活性劑,即使在長期運作下,該有機無機奈米複合粒子仍可以穩定分散於該基礎潤滑油中,降低磨耗阻力。在該潤滑油組合物中,該有機/無機奈米複合粒子可具有一重量百分比係介於0.01%至2%(100ppm-20000ppm),以該潤滑油組合物的總重為基準;較佳者為該有機/無機奈米複合粒子係具有一重量百分比係介於0.15%至0.5%(1500ppm-5000ppm),以該潤滑油組合物的總重為基準。The present invention provides a lubricating oil composition comprising a base lubricating oil and an organic-inorganic nanodiamond composite particles uniformly dispersed in the base lubricating oil. The lubricating oil composition does not need to add any dispersing agent or surfactant, and the organic-inorganic nano composite particles can be stably dispersed in the base lubricating oil even under long-term operation, thereby reducing wear resistance. In the lubricating oil composition, the organic/inorganic nano composite particles may have a weight percentage of 0.01% to 2% (100 ppm to 20000 ppm) based on the total weight of the lubricating oil composition; preferably The organic/inorganic nanocomposite particle system has a weight percentage of from 0.15% to 0.5% (1500 ppm to 5000 ppm) based on the total weight of the lubricating oil composition.

該基礎潤滑油可包含:礦物油、齒輪油、半合成油、全合成油、削切油、油脂、或其混合。請參照第1圖,係為該有機/無機奈米複合粒子的解團聚體示意圖。由圖可知,該有機/無機奈米複合粒子10係為一表面具有接枝高分子鏈16的奈米鑽石顆粒12,其中該奈米鑽石顆粒其表面具有石墨層14,而該接枝高分子鏈16則係接枝於該石墨層14上,因此原奈米鑽石的團聚體,其大小由數個微米,因接枝高分子而解團聚成為由數顆有機/無機奈米複合粒子所組成的較小之解團聚體,其大小僅數十奈米。用來接枝於該奈米鑽石顆粒的高分子鏈,可為疏水性高分子,例如:聚甲基丙烯酸甲酯(polymethylmethacrylate、PMMA)、聚甲基丙烯酸缩水甘油酯(poly(glycidyl methylacrylate)、PGMA)、聚苯乙烯(polystyrene、PS)、或其混合。該高分子鏈主要可依據基礎潤滑油的極性來進行選用及搭配,使鍵結有該接枝高分子鏈的奈米鑽石能完全分散並長期穩定於潤滑油中。該有機/無機奈米複合粒子的平均粒徑可為10nm至250nm。對於該有機/無機奈米複合粒子,該接枝高分子鏈可佔該有機/無機奈米複合粒子的總量的4wt%至50wt%;較佳為15wt%至.40wt%。The base lubricating oil may comprise: mineral oil, gear oil, semi-synthetic oil, fully synthetic oil, cut oil, grease, or a mixture thereof. Please refer to Fig. 1 for a schematic diagram of the deagglomeration of the organic/inorganic nano composite particles. As can be seen from the figure, the organic/inorganic nano composite particle 10 is a nano diamond particle 12 having a grafted polymer chain 16 on the surface thereof, wherein the nano diamond particle has a graphite layer 14 on its surface, and the graft polymer The chain 16 is grafted onto the graphite layer 14, so that the agglomerates of the original nano-diamonds are several micrometers in size, and are agglomerated by the grafting polymer to form a composite of several organic/inorganic nano composite particles. The smaller solution agglomerates, which are only a few tens of nanometers in size. The polymer chain used for grafting to the nanodiamond particles may be a hydrophobic polymer such as polymethylmethacrylate (PMMA) or poly(glycidyl methylacrylate). PGMA), polystyrene (PS), or a mixture thereof. The polymer chain can be selected and matched according to the polarity of the base lubricating oil, so that the nano-diamond bonded with the grafted polymer chain can be completely dispersed and stably stabilized in the lubricating oil for a long time. The organic/inorganic nano composite particles may have an average particle diameter of 10 nm to 250 nm. For the organic/inorganic nano composite particles, the graft polymer chain may constitute 4% by weight to 50% by weight of the total of the organic/inorganic nano composite particles; preferably 15% by weight to 40% by weight.

該有機/無機奈米複合粒子的製備方式包含以下步驟:首先,將一奈米鑽石顆粒(例如超分散奈米鑽石)與一反應單體混合,得到一混合物,其中該反應單體在後續一聚合過程會形成接枝於該奈米鑽石顆粒之高分子鏈,例如:甲基丙烯酸甲酯、甲基丙烯酸缩水甘油酯、苯乙烯、或其混合。上述混合物可進一步包含一溶劑,可為一般的極性溶劑如乙醇或丙酮,或非極性溶劑如甲苯,視其接枝單體的極性而定。接著,對該溶液進行一濕式球磨解團聚製程,且在球磨過程中並同時加入自由基起始劑以對該反應單體進行一聚合反應。換言之,本發明特點是讓奈米鑽石顆粒(例如超分散奈米鑽石)解團聚並同時於其表面鍵結接枝高分子(由反應單體聚合而成)。該濕式球磨解團聚製程係使用鋯珠來進行球磨,其中該鋯珠具有一粒徑尺寸介於15至200微米之間,且所加入的鋯珠與欲進行球磨的奈米鑽石具有一重量比介於40:1至400:1之間。該自由基起始劑可為過氧化物起始劑或是偶氮化合物起始劑,例如二乙氧基苯乙酮(diethoxy acetophenone)、二苯甲酮(benzophenone)、苯基安息香異丁醚(benzyl benzoin isobutyl ether)、苯二甲基醇縮酮(benzyl dimethyl ketal)、1-羥環己基苯基丙酮(1-hydroxycyclohexyl phenyl ketone)、二乙基塞吨酮(diethyl thioxanthone)、2-乙基蒽醌(2-ethyl anthraquinone)、2-羥基-2-甲基-1-苯基丙烷-1-酮(2-hydroxy-2-methyl-1-phenylpropane-1-one)、1-(4-異丙基苯基)-2-羥基-2-甲基丙烷-1-酮(1-(4-isopropylphenyl)-2-hydroxy-2-methylpropane-1-one)、2-甲基-[4-(甲基硫)苯基]-2-嗎啉基-1-丙烷(2-methyl-[4-(meyhylthio)phenyl]-2-morpholino-1-propane)、芳香重偶氮鹽(aromatic diazonium salts)、三烯丙基銃鹽(triallysulfonium salts)、二烯丙基碘鹽(diallyiodonium salts)、路易士酸與金烯觸媒化合物之三烯丙基硒鹽(triallylselenium salts of Lewis acid as well as metallocene compounds)、或其混合。當能量施加於起始劑時,將使起始劑斷鍵形成自由基,進而使烯類單體聚合成高分子並接枝於奈米鑽石表面的石墨結構上。當高分子接枝於奈米鑽石的石墨表面時,將會使奈米鑽石更易分散於溶劑中並露出更多表面,使得其他未接枝之高分子更易接枝於奈米鑽石的石墨表面上。當奈米鑽石表面鍵結大量高分子後便完全分散並溶於溶劑中。該濕式球磨解團聚製程的機械球磨速率可介於10-20m/s,球磨時間可為數小時。The preparation method of the organic/inorganic nano composite particles comprises the following steps: First, a nanometer diamond particle (for example, a super-dispersed nano diamond) is mixed with a reactive monomer to obtain a mixture, wherein the reaction monomer is in the subsequent one. The polymerization process forms a polymer chain grafted to the nanodiamond particles, such as methyl methacrylate, glycidyl methacrylate, styrene, or a mixture thereof. The above mixture may further comprise a solvent which may be a general polar solvent such as ethanol or acetone, or a non-polar solvent such as toluene, depending on the polarity of the graft monomer. Next, the solution is subjected to a wet ball milling agglomeration process, and a radical initiator is simultaneously added during the ball milling to carry out a polymerization reaction on the reaction monomer. In other words, the present invention is characterized in that a nano-diamond particle (for example, a super-dispersed nano-diamond) is deagglomerated and a graft polymer (polymerized from a reactive monomer) is bonded to the surface thereof. The wet ball milling agglomeration process uses a zirconium bead for ball milling, wherein the zirconium bead has a particle size between 15 and 200 microns, and the added zirconium beads have a weight with the nanodiamond to be ball milled. The ratio is between 40:1 and 400:1. The radical initiator may be a peroxide initiator or an azo compound initiator, such as diethoxy acetophenone, benzophenone, phenylbenzoin isobutyl ether (benzyl benzoin isobutyl ether), benzyl dimethyl ketal, 1-hydroxycyclohexyl phenyl ketone, diethyl thioxanthone, 2-B 2-ethyl anthraquinone, 2-hydroxy-2-methyl-1-phenylpropane-1-one, 1-(4) -isopropylphenyl)-2-hydroxy-2-methylpropan-1-one (1-(4-isopropylphenyl)-2-hydroxy-2-methylpropane-1-one), 2-methyl-[4 -(methylthio)phenyl]-2-morpholino-1-propane (2-methyl-[4-(meyhylthio)phenyl]-2-morpholino-1-propane), aromatic azozonium (aromatic azozonium) Salts, trially sulfonium salts, diallyiodonium salts, triallylselenium salts of Lewis acid as well as Metallocene compounds), or a mixture thereof. When energy is applied to the starter, the initiator is broken to form a radical, which in turn polymerizes the vinyl monomer into a polymer and grafts onto the graphite structure on the surface of the nanodiamond. When the polymer is grafted onto the graphite surface of the nano-diamond, the nano-diamond will be more easily dispersed in the solvent and expose more surface, so that other ungrafted polymers are more easily grafted onto the graphite surface of the nano-diamond. . When the surface of the nano-diamond is bonded to a large amount of polymer, it is completely dispersed and dissolved in the solvent. The wet ball agglomeration process can have a mechanical ball milling rate of 10-20 m/s and a ball milling time of several hours.

接著,將奈米鑽石以高速離心方式沉澱下來,並將未鍵結的高分子去除掉,之後加入溶劑再分散奈米鑽石,反覆重覆上述離心及分散步驟後,可完全去除去未鍵結的高分子。Next, the nano-diamond is precipitated by high-speed centrifugation, and the unbonded polymer is removed, and then the solvent is added to redisperse the nano-diamond, and after repeating the above-mentioned centrifugation and dispersion steps, the unbonded portion can be completely removed. Polymer.

本發明所述之潤滑油組合物的製備方法,除了包括上述製備該有機/無機奈米複合粒子的步驟外,更包括將該有機/無機奈米複合粒子與該基礎潤滑油混合,並進行一分散程序。該分散程序可為20千赫至40千赫的超音波振盪、60轉/分鐘至10000轉/分鐘的球磨、或上述之組合。若超音波振盪的頻率過低或球磨轉速過慢,則無法將奈米鑽石有效分散於溶劑中。若超音波振盪的頻率過高或球磨轉速過快,則容易導致局部溫度過熱使有機化合物降解,反而降低其效果。The method for preparing the lubricating oil composition of the present invention comprises, in addition to the above steps of preparing the organic/inorganic nano composite particles, further comprising mixing the organic/inorganic nano composite particles with the base lubricating oil, and performing one Decentralized procedure. The dispersion procedure may be an ultrasonic oscillation of 20 kHz to 40 kHz, a ball milling of 60 rpm to 10,000 rpm, or a combination thereof. If the frequency of the ultrasonic oscillation is too low or the ball milling speed is too slow, the nano diamond cannot be effectively dispersed in the solvent. If the frequency of the ultrasonic oscillation is too high or the rotational speed of the ball mill is too fast, it is easy to cause local temperature overheating to degrade the organic compound, and the effect is lowered.

為了讓本發明之上述和其他目的、特徵、和優點能更明顯易懂,下文特舉數實施例配合所附圖式,作詳細說明如下:The above and other objects, features and advantages of the present invention will become more apparent and understood.

有機/無機奈米複合粒子的製備Preparation of organic/inorganic nano composite particles

實施例1Example 1

混合400公克的氧化鋯球(粒徑約50μm)與10公克的超分散奈米鑽石(商品編號為UDD,購自伯罕企業有限公司ABBA group,係以密閉爆炸方式並經過酸洗去除雜質所製備),並加入80g之甲基丙烯酸甲酯單體,所得之混合物置於一球磨腔槽中。球磨腔槽外部循環水溫設定80℃,球磨轉速設定為每分鐘2400轉。最後將10克的自由基起始劑過氧化苯(benzoyl peroxide)溶於10毫升的甲苯,在球磨過程中以流速約小時5毫升速度注入腔槽裡。利用球磨方式將團聚奈米鑽石分散,同時由過氧化苯產生單體聚合反應的自由基加成在奈米鑽石表面上,讓奈米鑽石逐漸接枝高分子,並逐漸穩定分散於溶劑。高分子接枝在奈米鑽石表面上,因而慢慢分散於溶劑中而曝露更多表面,使得更多高分子可接枝在奈米鑽石表面上。最後,高速離心將奈米鑽石接枝高分子離心下來,把未接枝的高分子及溶劑去除掉,經過反覆以甲苯清洗後便得到接枝聚高分子的奈米鑽石-奈米鑽石接枝聚甲基丙烯酸甲酯(UDD-PMMA)。請參照第2圖,係為該奈米鑽石接枝聚甲基丙烯酸甲酯之紅外線吸收光譜圖。如圖所示,該紅外線吸收光譜圖除了具有C-H鍵伸縮(carbon-hydrogen stretching)的吸收如-2980和2932 cm-1 ,以及較低頻率C-H鍵伸縮(carbon-hydrogen stretching)的吸收如1430-1470 cm-1 區域(証明官能基團具有亞甲基結構)外,更具有特徵酯類的C=O振動的強吸收如1725cm-1 ,及酯類特徵的C-O伸縮的強吸收帶如1050-1300cm-1Mix 400 g of zirconia balls (particle size about 50 μm) with 10 g of ultra-dispersed nano-diamonds (product number UDD, purchased from ABBA group of Bakhan Enterprise Co., Ltd., in a closed explosion and acid-washed to remove impurities) Prepare) and add 80 g of methyl methacrylate monomer, and the resulting mixture is placed in a ball mill chamber. The external circulating water temperature of the ball mill chamber is set to 80 ° C, and the ball mill speed is set to 2,400 rpm. Finally, 10 g of the free radical initiator benzoyl peroxide was dissolved in 10 ml of toluene and injected into the chamber at a flow rate of about 5 ml at a flow rate during the ball milling process. The agglomerated nano-diamonds are dispersed by ball milling, and the free radical addition of monomer polymerization by benzoyl peroxide is applied to the surface of the nano-diamonds, so that the nano-diamonds are gradually grafted with the polymer and gradually dispersed in the solvent. The polymer is grafted onto the surface of the nano-diamond, and thus slowly dispersed in the solvent to expose more surface, so that more polymer can be grafted on the surface of the nano-diamond. Finally, high-speed centrifugation centrifuges the nano-diamond graft polymer, removes the ungrafted polymer and solvent, and after washing with toluene, the nano-diamond-nano diamond grafted with grafted polymer is obtained. Polymethyl methacrylate (UDD-PMMA). Please refer to Fig. 2 for the infrared absorption spectrum of the nano-diamond grafted polymethyl methacrylate. As shown, the infrared absorption spectrum has absorptions such as -20080 and 2932 cm -1 with carbon-hydrogen stretching, and absorption of lower-frequency carbon-hydrogen stretching such as 1430- In addition to the 1470 cm -1 region (proving that the functional group has a methylene structure), the strong absorption of the C=O vibration of the characteristic esters such as 1725 cm -1 , and the strong absorption band of the CO stretching of the ester characteristics such as 1050- 1300cm -1 .

接著,以熱重分析儀對該奈米鑽石接枝聚甲基丙烯酸甲酯進行分析,以評估奈米鑽石表面接枝的高分子的重量比率,結果如第3圖所示。由圖可知,大部份接枝的高分子會200℃-500℃產生熱分解,因而造成重量損失。以熱重損失分析來估計,表面高分子所佔比率約32%左右。該奈米鑽石接枝聚甲基丙烯酸甲酯以粒徑分析其粒徑分佈,結果如第5圖所顯示,其粒徑尺寸(d50)平均約~20nm左右。Next, the nano-diamond-grafted polymethyl methacrylate was analyzed by a thermogravimetric analyzer to evaluate the weight ratio of the polymer grafted on the surface of the nano-diamond, and the results are shown in Fig. 3. As can be seen from the figure, most of the grafted polymers will thermally decompose from 200 ° C to 500 ° C, resulting in weight loss. It is estimated by thermogravimetric loss analysis that the proportion of surface polymer is about 32%. The nano-diamond grafted polymethyl methacrylate was analyzed for particle size distribution by particle size. As a result, as shown in Fig. 5, the particle size (d50) averaged about -20 nm.

實施例2-3Example 2-3

實施例2及3分別如實施例1之相同方式進行,但分別以甲基丙烯酸缩水甘油酯及苯乙烯取代甲基丙烯酸甲酯作為反應單體。請參照第4圖,係為實施例2所得之奈米鑽石接枝聚甲基丙烯酸缩水甘油酯(UDD-PGMA)及實施例3所得之奈米鑽石接枝聚苯乙烯(UDD-PS)的紅外線吸收光譜圖。而第6圖係實施例2所得的奈米鑽石接枝聚甲基丙烯酸縮水甘油酯(UDD-PGMA)其粒徑分析,結果顯示平均粒徑(d50)約10nm左右。而圖7圍為實施例3所得的奈米鑽石接聚苯乙烯(UDD-PS)其粒徑分析,其結果顯示平均粒徑(d50)約100nm左右。Examples 2 and 3 were carried out in the same manner as in Example 1, except that methyl methacrylate and styrene were substituted for methyl methacrylate as reaction monomers, respectively. Please refer to FIG. 4 , which is the nano diamond graft polyglycidyl methacrylate (UDD-PGMA) obtained in Example 2 and the nano diamond-grated polystyrene (UDD-PS) obtained in Example 3. Infrared absorption spectrum. On the other hand, the particle size analysis of the nanodiamond graft polyglycidyl methacrylate (UDD-PGMA) obtained in Example 2 shows that the average particle diameter (d50) is about 10 nm. On the other hand, Fig. 7 is a particle size analysis of the nanodiamond-polystyrene (UDD-PS) obtained in Example 3, and as a result, the average particle diameter (d50) was about 100 nm.

潤滑油組合物的製備及性質量測Preparation and quality measurement of lubricating oil composition

實施例4Example 4

將實施例1所得之奈米鑽石接枝聚甲基丙烯酸甲酯以不同濃度(添加比例分別為0ppm、500ppm、1000ppm、1500ppm、2000ppm、及3000ppm)加入基礎潤滑油(商品編號為CPC R68、由中油製造販售)進行測試,以比較其磨擦係數、油溫和磨耗率(以翼對環(Vans-on-ring)方式模擬潤滑油在機件滑動時的磨耗試驗),結果顯示於表1。The nano-diamond grafted polymethyl methacrylate obtained in Example 1 was added to the base lubricating oil at different concentrations (addition ratios of 0 ppm, 500 ppm, 1000 ppm, 1500 ppm, 2000 ppm, and 3000 ppm, respectively) (product number is CPC R68, The oil production and sales were tested to compare the friction coefficient, oil temperature and wear rate (the vanes-on-ring method was used to simulate the abrasion test of the lubricant when the machine was sliding). The results are shown in Table 1.

此外,請參照第8圖,係顯示奈米鑽石接枝聚甲基丙烯酸甲酯添加量為0ppm、1000ppm、2000ppm、及3000ppm之潤滑油組合物其磨擦係數與時間的關係圖;請參照第9圖,係顯示奈米鑽石接枝聚甲基丙烯酸甲酯添加量為0ppm、1000ppm、2000ppm、及3000ppm之潤滑油組合物其油溫與時間的關係圖。Further, referring to Fig. 8, a graph showing the relationship between the friction coefficient and the time of the lubricating oil composition in which the amount of the nano diamond grafted polymethyl methacrylate is 0 ppm, 1000 ppm, 2000 ppm, and 3000 ppm is added; The graph shows the oil temperature versus time for a lubricating oil composition in which nano diamond grafted polymethyl methacrylate is added in amounts of 0 ppm, 1000 ppm, 2000 ppm, and 3000 ppm.

該磨擦係數、油溫和磨耗率詳細的測式方式說明如下:以磨耗測試機(Falex#6,USA)測試及數據擷取系統(Red Lion CSMSTRSX,USA)紀錄油溫和磨擦係數。選擇塊對環的模式作測試,是模擬內燃機中環形和圓筒活塞組件。翼對環的測試中塊狀結構為2.4mmx4.8mmx6.3mm長方形塊狀SKD11不鏽鋼,塊狀上試件以垂直滑動方向接觸環形試件,在測試前粗糙度Ra=0.044μm。整個磨耗試件浸入加滿潤滑油的油杯,並以滑動速率為6.08m/s,接觸壓力為4.33×106 Pa。磨擦係數及油溫以每秒紀錄一次,整個測試時間約4320秒,總滑動距離約為26283公尺。The detailed measurement of the friction coefficient, oil temperature and wear rate is as follows: The oil temperature and friction coefficient are recorded by the abrasion tester (Falex #6, USA) test and data acquisition system (Red Lion CSMSTRSX, USA). The block-to-ring mode was chosen to simulate the annular and cylindrical piston assemblies in an internal combustion engine. In the test of the wing-to-ring, the block structure was a 2.4 mm x 4.8 mm x 6.3 mm rectangular block of SKD11 stainless steel, and the test piece on the block contacted the annular test piece in a vertical sliding direction with a roughness Ra of 0.044 μm before the test. The entire abradable test piece was immersed in an oil cup filled with lubricating oil at a sliding rate of 6.08 m/s and a contact pressure of 4.33 x 10 6 Pa. The friction coefficient and oil temperature are recorded once per second. The entire test time is about 4320 seconds and the total sliding distance is about 26283 meters.

比較實施例1Comparative Example 1

混合400公克的氧化鋯球(粒徑約50μm)與10公克的超分散奈米鑽石(商品編號為UDD,購自伯罕企業有限公司ABBA group,係以密閉爆炸方式並經過酸洗去除雜質所製備),並加入約100ml溶劑四氫呋喃,所得之混合物置於一球磨腔槽中。球磨腔槽外部循環水溫設定80℃,球磨轉速設定為每分鐘2400轉。接著,將鋯球過篩後並去除掉溶劑,得到解團聚的奈米鑽石顆粒。最後,將所得之解團聚的奈米鑽石顆粒加入基礎潤滑油(商品編號為CPC R68、由中油製造販售)中(解團聚的奈米鑽石顆粒添加比例為2000ppm),並加入2%界面活性劑-油酸山梨糖醇酐(商品編號為Span80),以超音波震盪1小時,得到一潤滑油組合物。Mix 400 g of zirconia balls (particle size about 50 μm) with 10 g of ultra-dispersed nano-diamonds (product number UDD, purchased from ABBA group of Bakhan Enterprise Co., Ltd., in a closed explosion and acid-washed to remove impurities) Prepare) and add about 100 ml of solvent tetrahydrofuran, and the resulting mixture is placed in a ball mill chamber. The external circulating water temperature of the ball mill chamber is set to 80 ° C, and the ball mill speed is set to 2,400 rpm. Next, the zirconium balls are sieved and the solvent is removed to obtain deagglomerated nanodiamond particles. Finally, the obtained deagglomerated nanodiamond particles were added to the base lubricating oil (commercial number CPC R68, sold by CNPC) (the deagglomerated nanodiamond particles were added in a ratio of 2000 ppm), and 2% interfacial activity was added. The sorbitan oleate (commercial number is Span 80) was shaken for 1 hour with ultrasonic waves to obtain a lubricating oil composition.

接著,以與實施例4相同的方式量測比較實施例1所得之潤滑油組合物,並與實施例4所述之潤滑油組合物(奈米鑽石接枝聚甲基丙烯酸甲酯添加量為2000ppm)進行比較,結果顯示於表2。Next, the lubricating oil composition obtained in Comparative Example 1 was measured in the same manner as in Example 4, and the lubricating oil composition described in Example 4 (nano diamond grafted polymethyl methacrylate was added in an amount of 2000 ppm) was compared and the results are shown in Table 2.

此外,請參照第10圖,係顯示比較實施例1所得之潤滑油組合物與實施例4所述之潤滑油組合物(奈米鑽石接枝聚甲基丙烯酸甲酯添加量為2000ppm)其磨擦係數與時間的關係圖;請參照第11圖,係顯示比較實施例1所得之潤滑油組合物與實施例4所述之潤滑油組合物(奈米鑽石接枝聚甲基丙烯酸甲酯添加量為2000ppm)其油溫與時間的關係圖。由上兩圖可看出,雖然以界面活性分散奈米鑽石(比較實施例1所得之潤滑油組合物)於潤滑油初期具有很好潤滑效果,但隨著磨耗時間增加,潤滑效果慢慢降低,直到最後因奈米鑽石不穩定再次團聚成更大凝聚體造成其更嚴重刮損情況。反觀本發明所述之潤滑油組合物,以有機無機奈米鑽石複合粒子為潤滑油添加劑,可均勻且穩定的分散於潤滑基礎油中,因此具有較佳的潤滑效果及穩定性。Further, referring to Fig. 10, the lubricating oil composition obtained in Comparative Example 1 and the lubricating oil composition described in Example 4 (nano diamond grafted polymethyl methacrylate added in an amount of 2000 ppm) were rubbed. A graph showing the relationship between the coefficient and time; referring to Fig. 11, showing the lubricating oil composition obtained in Comparative Example 1 and the lubricating oil composition described in Example 4 (nano diamond grafted polymethyl methacrylate added) It is 2000 ppm) its oil temperature versus time. As can be seen from the above two figures, although the interfacially active dispersed nano-diamond (the lubricating oil composition obtained in Comparative Example 1) has a good lubricating effect at the initial stage of the lubricating oil, the lubricating effect is gradually lowered as the abrasion time increases. Until the final re-agglomeration of the nano-diamonds into larger aggregates caused more serious scratching. In contrast, the lubricating oil composition of the present invention uses the organic-inorganic nano-diamond composite particles as a lubricating oil additive, and can be uniformly and stably dispersed in the lubricating base oil, thereby having better lubricating effect and stability.

本發明所述之潤滑油組合物,相較其他專利文獻使用界面活性劑將奈米鑽石分散於潤滑油中的潤滑油組合物相比,具有以下優點:The lubricating oil composition of the present invention has the following advantages over the lubricating oil composition in which the surfactant is used to disperse the nanodiamond in the lubricating oil compared to other patent documents:

1.可更廣泛性應用於各種種類潤滑油、齒輪油、切削油和油脂。1. It can be used in a wide range of lubricants, gear oils, cutting oils and greases.

2.具有較長期穩定、耐熱性,因此在長期運作下仍不會有在團聚現象而保有潤滑特性。2. It has long-term stability and heat resistance, so it will not have agglomeration phenomenon and retain lubrication characteristics under long-term operation.

3.組成成分單純無須添加過多試劑影響潤滑油特性以致於影響其應用功能特性。3. The composition is purely without the need to add too much reagent to affect the properties of the lubricating oil so as to affect the functional properties of the application.

雖然本發明已以較佳實施例揭露如上,然其並非用以限定本發明,任何熟習此技藝者,在不脫離本發明之精神和範圍內,當可作些許之更動與潤飾,因此本發明之保護範圍當視後附之申請專利範圍所界定者為基準。While the present invention has been described in its preferred embodiments, the present invention is not intended to limit the invention, and the present invention may be modified and modified without departing from the spirit and scope of the invention. The scope of protection is based on the definition of the scope of the patent application.

10...有機/無機奈米複合粒子10. . . Organic/inorganic nano composite particles

12...奈米鑽石顆粒12. . . Nano diamond particles

14...石墨層14. . . Graphite layer

以及as well as

16...接枝高分子鏈16. . . Grafted polymer chain

第1圖係為本發明一實施例所述之有機/無機奈米複合粒子的解團聚體示意圖。Fig. 1 is a schematic view showing the deagglomeration of organic/inorganic nano composite particles according to an embodiment of the present invention.

第2圖係為未接枝的奈米鑽石(UDD)與實施例1所述之奈米鑽石接枝聚甲基丙烯酸甲酯(UDD-PMMA)之紅外線吸收光譜圖。Fig. 2 is an infrared absorption spectrum of the ungrafted nanodiamond (UDD) and the nanodiamond grafted polymethyl methacrylate (UDD-PMMA) described in Example 1.

第3圖係為未接枝的奈米鑽石(UDD)與實施例1所述之奈米鑽石接枝聚甲基丙烯酸甲酯(UDD-PMMA)之熱重分析圖。Figure 3 is a thermogravimetric analysis of the ungrafted nanodiamond (UDD) and the nanodiamond grafted polymethyl methacrylate (UDD-PMMA) described in Example 1.

第4圖係為實施例2所述之奈米鑽石接枝聚甲基丙烯酸缩水甘油酯(UDD-PGMA)及實施例3所述之奈米鑽石接枝聚苯乙烯(UDD-PS)之紅外線吸收光譜圖。Figure 4 is an infrared ray of the nano-diamond graft polyglycidyl methacrylate (UDD-PGMA) described in Example 2 and the nano-diamond-grafted polystyrene (UDD-PS) described in Example 3. Absorption spectrum.

第5圖為實施例1所述的納米鑽石接枝聚甲基丙烯酸甲酯(UDD-PMMA)的粒徑分析。Fig. 5 is a particle size analysis of the nanodiamond graft polymethyl methacrylate (UDD-PMMA) described in Example 1.

第6圖為實施例2所述的納米鑽石接枝聚甲基丙烯酸縮水甘油酯(UDD-PGMA)的粒徑分析。Fig. 6 is a particle size analysis of the nanodiamond graft polyglycidyl methacrylate (UDD-PGMA) described in Example 2.

第7圖為實施例3所述的納米鑽石接枝聚苯乙烯(UDD-PS)的粒徑分析。Fig. 7 is a particle size analysis of the nanodiamond grafted polystyrene (UDD-PS) described in Example 3.

第8圖係顯示不同奈米鑽石接枝聚甲基丙烯酸甲酯添加量的潤滑油組合物其磨擦係數與時間的關係圖。Fig. 8 is a graph showing the friction coefficient versus time for a lubricating oil composition in which different nanodiamond grafted polymethyl methacrylate is added.

第9圖係顯示不同奈米鑽石接枝聚甲基丙烯酸甲酯添加量的潤滑油組合物其潤滑油油溫與時間的關係圖。Fig. 9 is a graph showing the relationship between the lubricating oil temperature and the time of a lubricating oil composition in which a different amount of nano-diamond grafted polymethyl methacrylate is added.

第10圖係顯示比較實施例1所得之潤滑油組合物與實施例4所述之潤滑油組合物(奈米鑽石接枝聚甲基丙烯酸甲酯添加量為2000ppm)其磨擦係數與時間的關係圖。Fig. 10 is a graph showing the relationship between the friction coefficient of the lubricating oil composition obtained in Comparative Example 1 and the lubricating oil composition of Example 4 (the amount of nano-diamond grafted polymethyl methacrylate added is 2000 ppm) and time. Figure.

第11圖係顯示比較實施例1所得之潤滑油組合物與實施例4所述之潤滑油組合物(奈米鑽石接枝聚甲基丙烯酸甲酯添加量為2000ppm)其潤滑油油溫與時間的關係圖。Figure 11 is a graph showing the lubricating oil composition obtained in Comparative Example 1 and the lubricating oil composition described in Example 4 (nano diamond grafted polymethyl methacrylate added in an amount of 2000 ppm). Diagram of the relationship.

10...有機/無機奈米複合粒子10. . . Organic/inorganic nano composite particles

12...奈米鑽石顆粒12. . . Nano diamond particles

14...石墨層14. . . Graphite layer

16...接枝高分子鏈16. . . Grafted polymer chain

Claims (7)

一種潤滑油組合物,基本上由以下成份所組成:一基礎潤滑油;以及一均勻分散於該基礎潤滑油之有機/無機奈米複合粒子,其中該有機/無機奈米複合粒子係為一表面具有接枝高分子鏈的奈米鑽石顆粒,且該奈米鑽石顆粒其表面具有一石墨層,而該接枝高分子鏈係接枝於該石墨層上,其中該接枝高分子鏈具有一重量百分比介於4%至50%,以該有機/無機奈米複合粒子的總重為基準,且該接枝的高分子鏈包括聚甲基丙烯酸甲酯、聚甲基丙烯酸缩水甘油酯、聚苯乙烯或前述之組合。 A lubricating oil composition consisting essentially of: a base lubricating oil; and an organic/inorganic nano composite particle uniformly dispersed in the base lubricating oil, wherein the organic/inorganic nano composite particle is a surface a nano diamond particle having a graft polymer chain, wherein the nano diamond particle has a graphite layer on its surface, and the graft polymer chain is grafted onto the graphite layer, wherein the graft polymer chain has a The weight percentage is between 4% and 50%, based on the total weight of the organic/inorganic nano composite particles, and the grafted polymer chain includes polymethyl methacrylate, polyglycidyl methacrylate, and poly Styrene or a combination of the foregoing. 如申請專利範圍第1項所述之潤滑油組合物,其中該有機/無機奈米複合粒子具有一重量百分比係介於0.01%至2%,以該潤滑油組合物的總重為基準。 The lubricating oil composition of claim 1, wherein the organic/inorganic nanocomposite particles have a weight percentage of from 0.01% to 2% based on the total weight of the lubricating oil composition. 如申請專利範圍第1項所述之潤滑油組合物,其中該有機/無機奈米複合粒子的平均粒徑係為10nm至250nm。 The lubricating oil composition according to claim 1, wherein the organic/inorganic nano composite particles have an average particle diameter of 10 nm to 250 nm. 如申請專利範圍第1項所述之潤滑油組合物,其中該基礎潤滑油包含:礦物油、齒輪油、半合成油、全合成油、削切油、油脂、或其混合。 The lubricating oil composition of claim 1, wherein the base lubricating oil comprises: mineral oil, gear oil, semi-synthetic oil, total synthetic oil, cut oil, grease, or a mixture thereof. 如申請專利範圍第1項所述之潤滑油組合物,其中該接枝的高分子鏈係為疏水性高分子鏈。 The lubricating oil composition according to claim 1, wherein the grafted polymer chain is a hydrophobic polymer chain. 一種潤滑油組合物的製備方法,用以製備申請專利範圍第1項所述之潤滑油組合物,包括:將一奈米鑽石顆粒與一反應單體進行混合,得到一混合物; 對該混合物進行一濕式球磨解團聚製程及一聚合反應,以形成一表面具有接枝高分子鏈的奈米鑽石顆粒,其中該接枝高分子鏈具有一重量百分比介於4%至50%,以該表面具有接枝高分子鏈的奈米鑽石顆粒的總重為基準,且該接枝的高分子鏈包括聚甲基丙烯酸甲酯、聚甲基丙烯酸缩水甘油酯、聚苯乙烯或前述之組合;以及將該表面具有接枝高分子鏈的奈米鑽石顆粒與一基礎潤滑油混合,並進行一分散程序。 A method for preparing a lubricating oil composition for preparing the lubricating oil composition according to claim 1, comprising: mixing one nanometer diamond particles with a reactive monomer to obtain a mixture; Performing a wet ball milling agglomeration process and a polymerization reaction on the mixture to form a nano diamond particle having a graft polymer chain on the surface, wherein the graft polymer chain has a weight percentage of 4% to 50% And based on the total weight of the nano-diamond particles having a grafted polymer chain on the surface, and the grafted polymer chain comprises polymethyl methacrylate, polyglycidyl methacrylate, polystyrene or the foregoing a combination of the nanodiamond particles having a grafted polymer chain on the surface and a base lubricating oil, and performing a dispersion process. 如申請專利範圍第6項所述之潤滑油組合物的製備方法,其中該分散程序包括超音波振盪、球磨、或其組合。 The method of preparing a lubricating oil composition according to claim 6, wherein the dispersing process comprises ultrasonic vibration, ball milling, or a combination thereof.
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Publication number Priority date Publication date Assignee Title
TW200710216A (en) * 2005-08-03 2007-03-16 3M Innovative Properties Co Thermally conductive grease
US20080249229A1 (en) * 2007-03-27 2008-10-09 Lukehart Charles M Diamond polymer brushes
TW200927913A (en) * 2007-12-31 2009-07-01 Ind Tech Res Inst Lube oil compositions

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW200710216A (en) * 2005-08-03 2007-03-16 3M Innovative Properties Co Thermally conductive grease
US20080249229A1 (en) * 2007-03-27 2008-10-09 Lukehart Charles M Diamond polymer brushes
TW200927913A (en) * 2007-12-31 2009-07-01 Ind Tech Res Inst Lube oil compositions

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