CN114015491B - 一种含改性纳米碳材料的润滑油添加剂及其制备方法 - Google Patents
一种含改性纳米碳材料的润滑油添加剂及其制备方法 Download PDFInfo
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- CN114015491B CN114015491B CN202111393250.2A CN202111393250A CN114015491B CN 114015491 B CN114015491 B CN 114015491B CN 202111393250 A CN202111393250 A CN 202111393250A CN 114015491 B CN114015491 B CN 114015491B
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- lubricating oil
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- oil additive
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- agent
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M167/00—Lubricating compositions characterised by the additive being a mixture of a macromolecular compound, a non-macromolecular compound and a compound of unknown or incompletely defined constitution, each of these compounds being essential
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/12—Preparation of carboxylic acid amides by reactions not involving the formation of carboxamide groups
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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
- C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
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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
- 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
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- C10M169/048—Mixtures of base-materials and additives the additives being a mixture of compounds of unknown or incompletely defined constitution, non-macromolecular and macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
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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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- C10M2201/041—Carbon; Graphite; Carbon black
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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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- C10M2201/066—Molybdenum sulfide
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- C—CHEMISTRY; METALLURGY
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- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M2201/00—Inorganic compounds or elements 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
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- C10M2203/1006—Petroleum or coal fractions, e.g. tars, solvents, bitumen used as base material
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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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- C10M2205/02—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers
- C10M2205/026—Butene
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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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- C10M2207/10—Carboxylix acids; Neutral salts thereof
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- C10M2207/125—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids
- C10M2207/126—Carboxylix acids; Neutral salts thereof having carboxyl groups bound to acyclic or cycloaliphatic carbon atoms having hydrocarbon chains of eight up to twenty-nine carbon atoms, i.e. fatty acids monocarboxylic
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Abstract
本发明公开了一种含改性纳米碳材料的润滑油添加剂，包括以质量分数计的改性纳米碳材料0.5～10wt％和助剂90～99.5wt％；所述的助剂包括：陶瓷相粉末1～5wt％，分散剂50～90wt％，清净剂0～10wt％，抗泡剂0～10wt％，极压抗磨剂1～5wt％，油性剂0.1～5wt％和黏度指数改进剂0.1～5wt％。优选的，所述的改性纳米碳材料为改性碳纳米管。所述的改性碳纳米管的比表面积大、分散性好，具有管壁空洞结构。将所述的含改性纳米碳材料的润滑油添加剂直接添加至商用润滑油中，能够改善润滑油的润滑性能和耐磨性能，降低机械摩擦面摩擦系数，修复磨损表面，提高机械寿命，延长换油周期，减少能源消耗。
Description
技术领域
本发明涉及润滑油添加剂的技术领域，尤其涉及一种含改性纳米碳材料的润滑油添加剂及其制备方法。
背景技术
润滑油添加剂对基础润滑油的性能至关重要，性能优异的润滑油添加剂可以改善润滑油的润滑性能，特别是摩擦磨损性能。据统计，每年约有30％的能源被摩擦消耗，约80％的零部件失效由磨损造成，因摩擦磨损造成的经济损失占到国家GDP的5％以上。面向应用于大型发动机等高端装备的新型超滑体系，不仅可以大幅降低其能耗、延长其使用寿命，还可以避免工作故障、提高机械安全。因此，超滑的原子尺度作用机理研究与超滑新体系的研制是减小摩擦降低能耗的有效手段之一。
纳米碳材料(特别是富勒烯、石墨烯和碳纳米管等)、纳米金属及其纳米硫化物颗粒具有巨大的润滑应用价值，它们都可以作为绿色高效的无机润滑添加剂，是传统有机添加剂的潜在的替代品。通常纳米材料的减磨机理分为：滚动轴承效应、形成保护膜机制、填充修复效应和抛光效应。研究表明富勒烯的减磨抗磨性能在碳材料中是比较优异的，减磨机理属于上述效应中的滚动轴承效应，但是富勒烯价格昂贵，成本较高。碳纳米管的价格仅为富勒烯价格的1％，但未经改性的碳纳米管相互缠绕、容易沉降，分散性能较差。
公开号为CN105542905A的中国专利文献公开了一种润滑油添加剂，该润滑油添加剂包含以重量百分比计为0.1～23％的纳米碳球、0.1～25％的纳米氮化铝球、1～20％的粘度调整剂、1～33％的分散剂、1～28％的消泡剂及1～15％的油溶性有机二价金属。该润滑油添加剂可通过优异的润滑特性，填补引擎室裂缝，并降低机件间的相互摩擦力。
公开号为CN112961725A的中国专利文献公开了一种环保润滑油添加剂，由包含以下重量份的原料制成：基础油25～35份、纳米氧化铝6.2～8.6份、植物蜡5～9份、苯并三氮唑0.8～2.4份及石墨5.2～7.6份，其中，纳米氧化铝具备良好的耐磨性能，且其粒径较小，能够填充在摩擦表面的凹痕内，改善摩擦表面的摩擦系数，此外纳米氧化铝在摩擦过程中会产生静电吸附作用，在摩擦表面形成保护膜，提升了润滑油的润滑性能。
发明内容
本发明提供了一种含改性纳米碳材料的润滑油添加剂，制备方法简单，能够改善润滑油的润滑性能和耐磨性能，降低机械摩擦面摩擦系数，修复磨损表面，提高机械寿命，减少能源消耗。
具体采用的技术方案如下：
一种含改性纳米碳材料的润滑油添加剂，包括以质量分数计的改性纳米碳材料0.5～10wt％和助剂90～99.5wt％；所述的助剂包括：陶瓷相粉末1～5wt％，分散剂50～90wt％，清净剂0～10wt％，抗泡剂0～10wt％，极压抗磨剂1～5wt％，油性剂0.1～5wt％和黏度指数改进剂0.1～5wt％。
优选的，所述的改性纳米碳材料为改性碳纳米管。
所述的改性碳纳米管的制备方法包括以下步骤：将碳纳米管加入到活化剂中混合均匀，保温处理得到浆料，洗涤并调pH值至中性，干燥后得到活化的碳纳米管；活化的碳纳米管经热处理后加入至氧化剂中，洗涤并调pH值至中性，干燥后得到固体物质，将固体物质加入到离子液体中，得到改性碳纳米管。
本发明通过活化、氧化处理在碳纳米管的管壁上凿孔，增大其比表面积后再用离子液体进行修饰，在碳纳米管的活性位点接枝离子，利用离子间的斥力来避免碳纳米管的互相缠绕，从而提高碳纳米管的分散性。此外，由于比表面积的增加，改性碳纳米管更易于在分散剂中分散，同时由于改性碳纳米管的管壁空洞的存在使其在摩擦副中被挤压时更易变形回弹，可基于滚动轴承效应和填充修复效应减少摩擦。
优选的，所述的活化剂为KOH溶液、ZnCl2溶液和H3PO4溶液中至少一种；所述的氧化剂为HNO3和HCl的混合物；所述的离子液体为AlCl3型离子液体，由AlCl3与N,N-二甲基乙酰胺(DMA)、N-甲基乙酰胺(NMA)或乙酰胺(AcA)为原料制得，包括：DMA-1.8AlCl3、DMA-1.5AlCl3、DMA-1.0AlCl3、NMA-2AlCl3、AcA-2AlCl3。
优选的，所述的碳纳米管的加入量为0.5～10wt％；所述的保温条件为4～6h，50～100℃；热处理后的碳纳米管与氧化剂的配比为1:6～8。
进一步优选的，所述的热处理的条件为：常压，200～400℃，1～5h。活化处理后的碳纳米管在热处理过程中更易断裂从而更有利于离子的接枝，碳纳米管接枝同种电荷离子，纳米分子间产生斥力从而改善了碳纳米管的分散性能，使其更易于在分散剂中分散。
优选的，所述的陶瓷相粉末为纳米金刚石、硫化钼。
进一步优选的，所述的硫化钼的粒径小于30nm，所述的纳米金刚石的粒径小于100nm。
优选的，所述的分散剂为油酸、span-80、环卞胺、十六烷基三甲基溴化铵和十二烷基硫酸钠中的至少一种。
优选的，所述的清净剂为磺酸盐或水杨酸盐中的一种或两种。清净剂可在发动机油路的金属表面形成一层分子保护膜，防止沉积物在金属表面聚集，起到保持清洁的作用；还可将已形成的沉积物的微小颗粒包围起来，形成油溶性胶束，分散到油中，随油燃烧，达到清洗的目的。
优选的，所述的抗泡剂为三烷基三聚氰胺、氰脲酰氯三聚氰胺、脂肪胺中的至少一种。抗泡剂的作用主要是抑制泡沫的产生，提高消除泡沫的速度。
优选的，所述的极压抗磨剂包括偏硼酸钠、偏硼酸钾、三硼酸钾、磷酸三甲酚酯、磷酸三苯酯、磷酸三乙酯、磷酸三丁酯和亚磷酸二正丁酯中的至少一种。极压抗磨剂可以缓和液体油膜被破坏。
优选的，所述的油性剂包括棕榈酸、油酸、月桂醇、鲸蜡醇、油脂、硬脂酸丁酯、鲸蜡基胺、油酰胺、酸式磷酸月桂酯、酸式磷酸油酰酯、硫化抹香鲸油和硫化油酸中的至少一种。
优选的，所述的粘度指数改进剂包括氢化苯乙烯双烯共聚物、聚异丁烯中的至少一种。
本发明还提供了所述的含改性纳米碳材料的润滑油添加剂的制备方法，所述的含改性纳米碳材料的润滑油添加剂由改性纳米碳材料与助剂调合得到。
优选的，调合工艺采用高压均质机或高速乳化机，转速500～4000rpm，时间20～180min。
与现有技术相比，本发明的有益效果在于：
(1)本发明制得的改性纳米碳材料的比表面积大、分散性好，具有管壁空洞结构，在摩擦副中被挤压时更易变形回弹，减磨效果优异。改性前碳纳米管的比表面积为141.53m2/g；改性后碳纳米管的比表面积达到396.47m2/g。
(2)本发明制得的含改性纳米碳材料的润滑油添加剂可直接添加至商用润滑油中，能够改善润滑油的润滑性能、耐磨性能和减磨性能，降低机械摩擦面摩擦系数，修复磨损表面，提高机械寿命，延长换油周期，减少能源消耗。
(3)本发明的含改性纳米碳材料的润滑油添加剂制备方法简单、原料易得，便于工业化生产。
附图说明
图1为对比例2中基础油的磨斑图片。
图2为实施例6中含所述润滑油添加剂的润滑油的磨斑图片。
图3为对比例2、实施例5、实施例3、对比例1产品的光学图片。
具体实施方式
下面结合附图与实施例，进一步阐明本发明。应理解，这些实施例仅用于说明本发明，而不用于限制本发明的范围。
实施例1～8中及对比例1～2中，基础油来源于壳牌15w，以多壁碳纳米管为纳米碳材料。
实施例1～8中，AlCl3型离子液体的合成方法为：DMA-2AlCl3合成方法：将13.34AlCl3(0.1mol)加入到N2保护的三口烧瓶，启动搅拌装置，将4.65mL DMA(0.05mol)缓慢滴加到三口烧瓶中，室温下搅拌30min；然后升至100℃后再继续搅拌反应3h，得到黄色透明的DMA-2AlCl3离子液体,存放于手套箱中备用。其他型离子液体DMA-1.8AlCl3、DMA-1.5AlCl3、DMA-1.0AlCl3、NMA-2AlCl3、AcA-2AlCl3按上述DMA-2AlCl3离子液体合成方法进行,其对应原料摩尔比为:
n(AlCl3):n(DMA)＝1.8:1；n(AlCl3):n(DMA)＝1.5:1,n(AlCl3):n(DMA)＝1:1；n(AlCl3):n(NMA)＝2:1；n(AlCl3):n(AcA)＝2:1。
将0.5wt％未改性碳纳米管加入到基础油中机械搅拌混合后作为对比例1，基础油作为对比例2。对比例2中，基础油的磨斑图片如图1所示，磨斑直径为0.421mm。
实施例1
(1)改性碳纳米管的制备
将碳纳米管加入到KOH活化剂中混合均匀，碳纳米管加入量为3.5wt％，60℃保温4h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤剩余的活化剂及活化过程中产生的杂质，并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经200℃、1.5h热处理后加入至氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:6)，4500r/min离心10min后过滤，用去离子水洗涤去除剩余的氧化剂及氧化过程中产生的杂质，调节pH值至中性后干燥得到固体物质，将固体物质加入到NMA-2AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将0.5wt％步骤(1)制得的改性碳纳米管、1wt％纳米金刚石、87.3wt％油酸分散剂、10wt％三烷基三聚氰胺抗泡剂、1wt％磷酸三苯酯极压抗磨剂、0.1wt％油酰胺(油性剂)、0.1wt％聚异乙烯粘度指数改进剂加入高速乳化机调合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
实施例2
(1)改性碳纳米管的制备
将碳纳米管加入KOH活化剂中混合均匀，碳纳米管加入量为2.0wt％，70℃保温5h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经220℃、2.5h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:6.5)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到AcA-2AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将10wt％步骤(1)制得的改性碳纳米管、5wt％MoS2、60wt％油酸分散剂、10wt％磺酸钙清净剂、5wt％磷酸三苯酯极压抗磨剂、5wt％油酰胺(油性剂)、5wt％聚异乙烯粘度指数改进剂加入高速乳化机调合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
实施例3
(1)改性碳纳米管的制备
将碳纳米管加入KOH活化剂中混合均匀，碳纳米管加入量为1.5wt％，80℃保温6h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经300℃、2h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:7)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到NMA-2AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将10wt％步骤(1)制得的改性碳纳米管、5wt％MoS2、50wt％span-80分散剂、10wt％水杨酸钙清净剂、10wt％三烷基三聚氰胺抗泡剂、5wt％磷酸三苯酯极压抗磨剂、5wt％油酰胺(油性剂)、5wt％聚异乙烯粘度指数改进剂加入高速乳化机混合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
实施例4
(1)改性碳纳米管的制备
将碳纳米管加入ZnCl2活化剂中混合均匀，碳纳米管加入量为2.0wt％，80℃保温6h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经300℃、2.5h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:8)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到DMA-1.5AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将1wt％步骤(1)制得的改性碳纳米管、2wt％纳米金刚石、90wt％环卞胺分散剂、1wt％水杨酸钙清净剂、1wt％三烷基三聚氰胺抗泡剂、1.2wt％磷酸三苯酯极压抗磨剂、0.8wt％油酰胺(油性剂)、3wt％聚异乙烯粘度指数改进剂加入高速乳化机混合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
实施例5
(1)改性碳纳米管的制备
将碳纳米管加入ZnCl2活化剂中混合均匀，碳纳米管加入量为3.5wt％，95℃保温5.5h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经350℃、3h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:6.2)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到DMA-1.8AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将2wt％步骤(1)制得的改性碳纳米管、4wt％陶瓷相粉末纳米金刚石、75wt％油酸分散剂、5wt％水杨酸钙清净剂、5wt％三烷基三聚氰胺抗泡剂、3wt％磷酸三乙酯极压抗磨剂、4wt％油酰胺(油性剂)、2wt％聚异乙烯粘度指数改进剂加入高速乳化机混合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
实施例6
(1)改性碳纳米管的制备
将碳纳米管加入ZnCl2活化剂中混合均匀，碳纳米管加入量为4.5wt％，75℃保温4h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经350℃、4h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:7.5)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到DMA-1.0AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将4wt％的改性碳纳米管、3wt％MoS2和纳米金刚石、70wt％油酸分散剂、6wt％磺酸钙清净剂、7wt％三烷基三聚氰胺抗泡剂、4wt％磷酸三乙酯极压抗磨剂、2wt％油酰胺(油性剂)、4wt％聚异乙烯粘度指数改进剂加入高速乳化机混合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。含所述润滑油添加剂的润滑油的磨斑图片如图2所示，其磨斑直径为0.339mm，较对比例2的基础油磨斑直径减小20％左右，即所述润滑油添加剂改善了润滑性能和耐磨性能。
实施例7
(1)改性碳纳米管的制备
将碳纳米管加入ZnCl2活化剂中混合均匀，碳纳米管加入量为5.5wt％，100℃保温6h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经400℃、4h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:8)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到DMA-1.5AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将7wt％步骤(1)制得的改性碳纳米管、3.5wt％陶瓷相粉末MoS2、80wt％环卞胺分散剂、2wt％磺酸钙清净剂、2.5wt％三烷基三聚氰胺抗泡剂、1.5wt％磷酸三乙酯极压抗磨剂、1wt％油酰胺(油性剂)、2.5wt％聚异乙烯粘度指数改进剂加入高速乳化机混合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
实施例8
(1)改性碳纳米管的制备
将碳纳米管加入H3PO4活化剂中混合均匀，碳纳米管加入量为3.0wt％，65℃保温6h得到浆料，5000rpm/min离心10min，过滤，去离子水洗涤并调节pH值至中性后，干燥后得到活化的碳纳米管；活化的碳纳米管经400℃、5h热处理后加入氧化剂中(热处理后的碳纳米管与氧化剂的配比为1:8)，4500r/min离心10min后过滤，用去离子水洗涤并调节pH值至中性后干燥得到固体物质，将固体物质加入到DMA-1.5AlCl3离子液体中恒温搅拌3h后抽滤烘干，得到改性碳纳米管。
(2)润滑油添加剂的制备
将9wt％步骤(1)制得的改性碳纳米管、4.5wt％陶瓷相粉末MoS2、58wt％油酸分散剂、9wt％磺酸钙清净剂、9wt％三烷基三聚氰胺抗泡剂、2.5wt％磷酸三乙酯极压抗磨剂、3.5wt％油酰胺(油性剂)、4.5wt％聚异乙烯粘度指数改进剂加入高速乳化机混合，转速3000rpm，乳化时间45min，得到含改性纳米碳材料的润滑油添加剂。
将该润滑油添加剂加入到基础油中，在机械搅拌调合器内搅拌调和45min，测试该润滑油添加剂的分散性和稳定性及产品的摩擦学行为。
样品分析
对比例2、实施例5、实施例3、对比例1产品的光学图片如图3所示，对比例2为基础油，由图看出比较澄清；对比例1中加入了浓度为0.5wt％未改性处理的碳纳米管后分散性能较差，出现轻微沉降；实施例5中加入了浓度为2wt％改性处理的碳纳米管后分散性能较好，分散均匀未出现沉降；实施例3中加入了浓度为10wt％改性处理的碳纳米管后分散均匀依然未出现沉降；即改性处理的碳纳米管分散性能较好。
采用四球机测试对比例1～2及实施例1～8的产品的摩擦学行为，测试条件为：试验条件为75℃，392N，转速为1200rpm，运行时间为3600s，磨斑直径结果如表1所示。
采用分光光度计在波长450nm处测试对比例1～2及实施例1～8的产品的吸光值，结果如表1所示。
表1对比例1～2及实施例1～8产品的性能测试
由表1数据可知，改性纳米碳材料不仅可改善基础油的抗磨减磨性能还可以大幅度提高碳材料在润滑油中的分散性。
此外，通过内燃发动机台架实验，较对比例2而言，实施例1～8的产品可节省燃油5％以上，节能效果显著。
以上所述的实施例对本发明的技术方案进行了详细说明，应理解的是以上所述的仅为本发明的具体实施例，并不用于限制本发明，凡在本发明的原则范围内所做的任何修改、补充或类似方式替代等，均应包含在本发明的保护范围之内。
Claims (9)
1.一种含改性纳米碳材料的润滑油添加剂，其特征在于，包括：
以质量分数计的改性纳米碳材料0.5~10 wt%和助剂90~99.5 wt%；
所述的助剂包括：陶瓷相粉末1~5 wt%，分散剂50~90 wt%，清净剂0~10 wt%，抗泡剂0~10 wt%，极压抗磨剂1~5 wt%，油性剂0.1~5 wt%和黏度指数改进剂0.1~5 wt%；
所述的改性纳米碳材料为改性碳纳米管，所述的改性碳纳米管的制备方法包括以下步骤：将碳纳米管加入到活化剂中混合均匀，保温处理得到浆料，洗涤并调pH值至中性，干燥后得到活化的碳纳米管；活化的碳纳米管经热处理后加入至氧化剂中，洗涤并调pH值至中性，干燥后得到固体物质，将固体物质加入到离子液体中，得到改性碳纳米管；
所述的活化剂为KOH溶液、ZnCl2溶液和H3PO4溶液中至少一种；所述的氧化剂为HNO3和HCl的混合物；所述的离子液体为AlCl3型离子液体，由AlCl3与N,N-二甲基乙酰胺、N-甲基乙酰胺或乙酰胺为原料制得。
2.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的碳纳米管的加入量为0.5~10 wt%；热处理后的碳纳米管与氧化剂的配比为1: 6~8。
3.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的陶瓷相粉末为纳米金刚石或硫化钼。
4.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的分散剂为油酸、span-80、环卞胺、十六烷基三甲基溴化铵和十二烷基硫酸钠中的至少一种。
5.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的清净剂为磺酸盐或水杨酸盐中的一种或两种；所述的抗泡剂为三烷基三聚氰胺、氰脲酰氯三聚氰胺、脂肪胺中的至少一种。
6.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的极压抗磨剂包括偏硼酸钠、偏硼酸钾、三硼酸钾、磷酸三甲酚酯、磷酸三苯酯、磷酸三乙酯、磷酸三丁酯和亚磷酸二正丁酯中的至少一种。
7.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的油性剂包括棕榈酸、油酸、月桂醇、鲸蜡醇、油脂、硬脂酸丁酯、鲸蜡基胺、油酰胺、酸式磷酸月桂酯、酸式磷酸油酰酯、硫化抹香鲸油和硫化油酸中的至少一种。
8.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂，其特征在于，所述的黏度指数改进剂 包括氢化苯乙烯双烯共聚物、聚异丁烯中的至少一种。
9.根据权利要求1所述的含改性纳米碳材料的润滑油添加剂的制备方法，其特征在于，所述的含改性纳米碳材料的润滑油添加剂由改性纳米碳材料与助剂调合得到。
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