新型无硫磷有机钼添加剂的制备与摩擦学性能研究
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摘要
近年来,为了节省能源和提高燃料的经济性,对润滑油添加剂的性能要求越来越高,同时,环保要求又对润滑油提出了无(低)硫磷的要求,保护尾气的三元催化装置,降低二烷基二硫代磷酸锌添加剂的使用量和取代二烷基二硫代磷酸锌已是必然。因此研究开发“无硫磷”、“无锌”润滑油添加剂和探索其摩擦磨损机理有很重要的理论价值和实用价值。
本课题从环保、节能、低投入及材料磨损的角度出发,以国内资源丰富、耐磨寿命最长和长期性能好的钼与不同碳链的羧酸为原料,合成了五种水溶性无硫磷有机钼添加剂和两种油溶性无硫磷有机钼添加剂,利用红外光谱对其结构进行表征。
文中对5种含钼水基润滑液采用四球机综合评定了承载能力、抗烧结能力和长时间摩擦磨损性能,端面试验机测试其对钢/紫铜、钢/铝摩擦副的摩擦磨损性能,疲劳试验机检测其耐疲劳寿命,结果表明,5种水溶性无硫磷有机钼添加剂均能大幅度提高水的承载能力、抗磨减摩性能;对钢/紫铜、钢/铝摩擦副均有较好的抗磨减摩性能;同时具有较好的抗疲劳性能。其中,a5的综合性能最好。
文中采用四球机综合评定了两种油溶性无硫磷有机钼(b1、b2)与市场产品ZDDP、MoDTP的承载能力和长时间摩擦磨损性能。试验结果表明,b1、b2的承载能力不如ZDDP和MoDTP,但抗磨减摩性能优于ZDDP和MoDTP;其中3%b1的抗磨减摩性能最好,摩擦系数和磨斑分别比150SN提高了51%和48%;无硫磷有机钼与T203有较好的抗磨减摩协同性;无硫磷有机钼对CF-4再生油也有较好的极压减摩抗磨效果。
对无硫磷有机钼化合物的摩擦磨损机理进行探讨,分析结果表明,无硫磷有机钼化合物在摩擦过程中与摩擦副表面发生化学反应,生成一层主要由有机氮吸附膜和铁的氧化物、三氧化钼沉积膜组成的边界复合润滑膜,从而起到了较好的极压减摩抗磨作用。
The issues of environment and energy sources have become international hotspots nowadays. And, environment regulations have been introduced to restrict the permissible level of phosphorus and sulphur (PS) because these can poison the catalysts that are used to remove pollutants from engine exhaust gas. These restrictions are leading to the development of low or zero PS additives which necessitate a reduction in the level of ZDDP employed in crankcase oils. So far, considerable study has been made by research institutions and additive companies to replace ZDDPs by another highly cost-effective compound, but the efforts have proved of little avail.
Molybdenum is well known for its lamella-layered structure and low-shear strength that provide excellent friction reduction characteristics in high-pressure contacts. In this study five kinds of water-soluble molybdenum-containing substitutes (WMCS) and two kinds of oil-soluble molybdenum-containing substitutes (OMCS) were synthesized by means of chemical reactions between a molybdenum source and a fatty acid salt of ethanol amine, and then characterized by FT-IR.
The four ball test results showed that all WMCS had obvious beneficial effect on the improvement of water lubricity; the results of end-face friction and wear tester on the steel/aluminum and steel/red copper friction pairs show that the WMCS have good impact on reducing the friction coefficient and wear; the results of fatigue test show that WMCS have good anti- fatigue properties. Thereof, a5 has the best over-all properties.
The four-ball tribotest results exhibited that the carrying capacity of b1, b2 is worse than that of ZDDP and MoDTP, but the friction-reduction and antiwear of b1, b2 are better. There into the average friction coefficient and WSD of b1 with concentration of 3.0% are the lowest of all, which are lower than 150SN base oil up to 51%, 48% respectively. What’s more, the SP-free organic molybdenum compounds can exhibit good antiwear and friction- reducing synergism with ZDDP.
The mechanism of extreme-pressure,antiwear and friction-reducing by these SP- free organic molybdenum compounds have also been discussed,showing that on the rubbing surface a protective film consisting of a reaction layer (FeO, Fe2O3 and FeOOH), a complicated organic nitrogen adsorption film and a sediment film MoO3 was formed as a result of decomposition of SP- free organic molybdenum.
本课题从环保、节能、低投入及材料磨损的角度出发,以国内资源丰富、耐磨寿命最长和长期性能好的钼与不同碳链的羧酸为原料,合成了五种水溶性无硫磷有机钼添加剂和两种油溶性无硫磷有机钼添加剂,利用红外光谱对其结构进行表征。
文中对5种含钼水基润滑液采用四球机综合评定了承载能力、抗烧结能力和长时间摩擦磨损性能,端面试验机测试其对钢/紫铜、钢/铝摩擦副的摩擦磨损性能,疲劳试验机检测其耐疲劳寿命,结果表明,5种水溶性无硫磷有机钼添加剂均能大幅度提高水的承载能力、抗磨减摩性能;对钢/紫铜、钢/铝摩擦副均有较好的抗磨减摩性能;同时具有较好的抗疲劳性能。其中,a5的综合性能最好。
文中采用四球机综合评定了两种油溶性无硫磷有机钼(b1、b2)与市场产品ZDDP、MoDTP的承载能力和长时间摩擦磨损性能。试验结果表明,b1、b2的承载能力不如ZDDP和MoDTP,但抗磨减摩性能优于ZDDP和MoDTP;其中3%b1的抗磨减摩性能最好,摩擦系数和磨斑分别比150SN提高了51%和48%;无硫磷有机钼与T203有较好的抗磨减摩协同性;无硫磷有机钼对CF-4再生油也有较好的极压减摩抗磨效果。
对无硫磷有机钼化合物的摩擦磨损机理进行探讨,分析结果表明,无硫磷有机钼化合物在摩擦过程中与摩擦副表面发生化学反应,生成一层主要由有机氮吸附膜和铁的氧化物、三氧化钼沉积膜组成的边界复合润滑膜,从而起到了较好的极压减摩抗磨作用。
The issues of environment and energy sources have become international hotspots nowadays. And, environment regulations have been introduced to restrict the permissible level of phosphorus and sulphur (PS) because these can poison the catalysts that are used to remove pollutants from engine exhaust gas. These restrictions are leading to the development of low or zero PS additives which necessitate a reduction in the level of ZDDP employed in crankcase oils. So far, considerable study has been made by research institutions and additive companies to replace ZDDPs by another highly cost-effective compound, but the efforts have proved of little avail.
Molybdenum is well known for its lamella-layered structure and low-shear strength that provide excellent friction reduction characteristics in high-pressure contacts. In this study five kinds of water-soluble molybdenum-containing substitutes (WMCS) and two kinds of oil-soluble molybdenum-containing substitutes (OMCS) were synthesized by means of chemical reactions between a molybdenum source and a fatty acid salt of ethanol amine, and then characterized by FT-IR.
The four ball test results showed that all WMCS had obvious beneficial effect on the improvement of water lubricity; the results of end-face friction and wear tester on the steel/aluminum and steel/red copper friction pairs show that the WMCS have good impact on reducing the friction coefficient and wear; the results of fatigue test show that WMCS have good anti- fatigue properties. Thereof, a5 has the best over-all properties.
The four-ball tribotest results exhibited that the carrying capacity of b1, b2 is worse than that of ZDDP and MoDTP, but the friction-reduction and antiwear of b1, b2 are better. There into the average friction coefficient and WSD of b1 with concentration of 3.0% are the lowest of all, which are lower than 150SN base oil up to 51%, 48% respectively. What’s more, the SP-free organic molybdenum compounds can exhibit good antiwear and friction- reducing synergism with ZDDP.
The mechanism of extreme-pressure,antiwear and friction-reducing by these SP- free organic molybdenum compounds have also been discussed,showing that on the rubbing surface a protective film consisting of a reaction layer (FeO, Fe2O3 and FeOOH), a complicated organic nitrogen adsorption film and a sediment film MoO3 was formed as a result of decomposition of SP- free organic molybdenum.
引文
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Bec S, Tonck A, Georges J M, Roper G W. Synergistic effects of MoDTC and ZDTP on frictional behaviour of tribofilms at the nanometer scale. Tribol. Lett. , 2004, 17: 797~809
Black A L, Dunsler R W, Sanders J V. Comparative study of surface deposites and behaviour of MoS2 particles and molybdenum dialkyl-dithio-phosphate. Wear, 1969, 119, 13~15
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Eugene V R, Thomas J K and Farmer H. Organic molybdenum complexs. US, 4889647, 1989
Farr J P. Molybdenum disulfide in lubrication-a review. Wear, 1975, 35: 1~25
Gatto V J, Devlin M T. Lubricant containing molybdenum compound and secondary diarylamine. US, 5650381, 1997
Hu J Q, Wei X Y, Yao J B, Han L, Zong Z M. Evaluation of molybdate ester as a synergist for arylamine antioxidant in lubricants. Tribol Int. 2006, 39 (11):1469~1473
Inoue K, Kurahashi T, Negishi T, Akiyama K, Ashimura K, Tasaka K. Effects of phosphorus and ash contents of engine oils on deactivation of monolithic three-way catalysts and oxygen sensors. SAE Technical Paper. 1992, 920654
Isoyama H, Sakurai T. The lubricating mechanisms of Diu-thiodithio-bis (diethyldithiocarbamate) dimolybdenum during extreme pPressure lubrication.Tribol Int. 1971, 7:151~160
Jain V K, Shukla D S. Study of the EP activity of water-soluble inorganic metallic salts for aqueous cutting fluids. Wear 1996, 193:226~234
Joby V J. Molybdenum-Sulfur Additives. US, 0132627, 2004
Kathryn C. Additives demand report projects small growth. Lubricants World, 2000, 10 (9): 24~25
Kumar S, Ferrari V, Burk P L, Deeba M, Rogalo J. Influence of phosphorus poisoning on TWCcatalysts. SAE Technical Paper. 2003, 01:3735
Ma H B, Li J, Yu Y, Zuo G Z, Ren T H. Tribological behaviors and film analysis of two ashless phosphorus/sulfur-containing additives in rapeseed oil. Acta Phys.Chim.Sin, 2008, 24 (5): 799~804
McFadden C S, Nicholas D S. Adsorption and surface chemistry in tribology. Tribology International, 1997, 30 (12): 881~ 888
Mould R W, Silver H B, Syrent R J. Investigation of the activity of oil additives. Part V the EP activity of some water-based fluids, Lub.Eng. , 1997, 33 (6): 291~298
Moritsugu K. Lubricating Oil Composition. US, 0082233, 2009
Rigney D A. Comments on the sliding wear of metals. Tribology International, 1997, 30 (5): 361~367
Shaub H. Mixed antioxidant composition. US, 6306803, 2001
Spikes H A. Tribology research in the twenty-first century. Tribology international, 2001, 34: 789~799
Spikes H A. Additive-additive and additive-surface interactions in lubrication. Lub.sci. 1989, 2 (1): 3~23
Szalontai G, Kiss G, Bartha L. Equilibria of mononuclear oxomolybdenum(VI) complexes of triethanolamine. A multinuclear dynamic magnetic resonance study of structure and exchange mechanisms. Spectrochim Acta, Part A 2003; 59: 1995~2007
Theo M. Wilfried D. Lubricants and Lubrication, German: Weinheim, 2001: 295~500
Unnikrishnan R, Jain M C, Harinarayan A K, Metha A K. Additive-additive interaction: an XPS study of the effect of ZDDP on the AW/EP characteristics of molybdenum based additives. Wear 2002, 252: 240~249
Vincent J G, Yvonne L B. The antioxidant properties of oraganomolybdenum compounds in engine oils. Tribology Lubrication Technology, 2003, (10): 40~ 47
Vincent J G, Edmund F P, Cheng K. Lubricants containing molybdenum compounds, phonates and diary amines. US, 61748421, 2001
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Wei D P, Song H Q. The Behavior of Steel lubricated by some Oxygen-containing Derivatives of Heterocyclic Nitrogen~containing Compounds (HNCC) under Boundary Lubrication Conditions. Lubrication Science, 1992, 4(3): 219~232
Wei D P, Song H Q, Wang R L. An investigation of the effects of some motor oil additives on the friction and wear behaviour of oil-soluble organomolybdenum compouds. Lubrication Science, 1991, 3(1):51~72
Wei D P, Spikes H A. The lubricity of diesel fuels. Wear, 1986, 111, 217~235
William R, Ruhe J R. Reduced Color Molybdenum-Containing Composition and a Method of Making same. US, 0324949, 2003
Winer W O. Future trends in tribology. Wear, 1990, 136: 19~27
Zheng P Y, Han X A, Wang R L. The mechanism of friction reduction of sulfurized oxymolybdenum di-(2-ethylhexyl)-phosphorodithioate under boundary lubrication. ASLE preprint No. 86-TC-4E-1
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Bec S, Tonck A, Georges J M, Roper G W. Synergistic effects of MoDTC and ZDTP on frictional behaviour of tribofilms at the nanometer scale. Tribol. Lett. , 2004, 17: 797~809
Black A L, Dunsler R W, Sanders J V. Comparative study of surface deposites and behaviour of MoS2 particles and molybdenum dialkyl-dithio-phosphate. Wear, 1969, 119, 13~15
Daniel G. Process for Preparation of Organo– Molybdenum Composition. US, 0070073, 2007 De V L, King J. Antioxidant combinations of molybdenum complexes and aromatic amine compounds. US, 4370246, 1983
Eugene V R, Thomas J K and Farmer H. Organic molybdenum complexs. US, 4889647, 1989
Farr J P. Molybdenum disulfide in lubrication-a review. Wear, 1975, 35: 1~25
Gatto V J, Devlin M T. Lubricant containing molybdenum compound and secondary diarylamine. US, 5650381, 1997
Hu J Q, Wei X Y, Yao J B, Han L, Zong Z M. Evaluation of molybdate ester as a synergist for arylamine antioxidant in lubricants. Tribol Int. 2006, 39 (11):1469~1473
Inoue K, Kurahashi T, Negishi T, Akiyama K, Ashimura K, Tasaka K. Effects of phosphorus and ash contents of engine oils on deactivation of monolithic three-way catalysts and oxygen sensors. SAE Technical Paper. 1992, 920654
Isoyama H, Sakurai T. The lubricating mechanisms of Diu-thiodithio-bis (diethyldithiocarbamate) dimolybdenum during extreme pPressure lubrication.Tribol Int. 1971, 7:151~160
Jain V K, Shukla D S. Study of the EP activity of water-soluble inorganic metallic salts for aqueous cutting fluids. Wear 1996, 193:226~234
Joby V J. Molybdenum-Sulfur Additives. US, 0132627, 2004
Kathryn C. Additives demand report projects small growth. Lubricants World, 2000, 10 (9): 24~25
Kumar S, Ferrari V, Burk P L, Deeba M, Rogalo J. Influence of phosphorus poisoning on TWCcatalysts. SAE Technical Paper. 2003, 01:3735
Ma H B, Li J, Yu Y, Zuo G Z, Ren T H. Tribological behaviors and film analysis of two ashless phosphorus/sulfur-containing additives in rapeseed oil. Acta Phys.Chim.Sin, 2008, 24 (5): 799~804
McFadden C S, Nicholas D S. Adsorption and surface chemistry in tribology. Tribology International, 1997, 30 (12): 881~ 888
Mould R W, Silver H B, Syrent R J. Investigation of the activity of oil additives. Part V the EP activity of some water-based fluids, Lub.Eng. , 1997, 33 (6): 291~298
Moritsugu K. Lubricating Oil Composition. US, 0082233, 2009
Rigney D A. Comments on the sliding wear of metals. Tribology International, 1997, 30 (5): 361~367
Shaub H. Mixed antioxidant composition. US, 6306803, 2001
Spikes H A. Tribology research in the twenty-first century. Tribology international, 2001, 34: 789~799
Spikes H A. Additive-additive and additive-surface interactions in lubrication. Lub.sci. 1989, 2 (1): 3~23
Szalontai G, Kiss G, Bartha L. Equilibria of mononuclear oxomolybdenum(VI) complexes of triethanolamine. A multinuclear dynamic magnetic resonance study of structure and exchange mechanisms. Spectrochim Acta, Part A 2003; 59: 1995~2007
Theo M. Wilfried D. Lubricants and Lubrication, German: Weinheim, 2001: 295~500
Unnikrishnan R, Jain M C, Harinarayan A K, Metha A K. Additive-additive interaction: an XPS study of the effect of ZDDP on the AW/EP characteristics of molybdenum based additives. Wear 2002, 252: 240~249
Vincent J G, Yvonne L B. The antioxidant properties of oraganomolybdenum compounds in engine oils. Tribology Lubrication Technology, 2003, (10): 40~ 47
Vincent J G, Edmund F P, Cheng K. Lubricants containing molybdenum compounds, phonates and diary amines. US, 61748421, 2001
Wagner C D. Handbook of X-ray photoelectron spectroscopy, PerkinElmer, Physical Electronic Division, MI, 1979.
Wei D P, Han X, Wang R L. The Influence of chemical structure of certain nitrogen-containingorganic compounds on their antiwear effectiveness~the critical role of Hydroxy Group. Lubrication Science, 1989, 2 (1): 63~87
Wei D P, Song H Q. The Behavior of Steel lubricated by some Oxygen-containing Derivatives of Heterocyclic Nitrogen~containing Compounds (HNCC) under Boundary Lubrication Conditions. Lubrication Science, 1992, 4(3): 219~232
Wei D P, Song H Q, Wang R L. An investigation of the effects of some motor oil additives on the friction and wear behaviour of oil-soluble organomolybdenum compouds. Lubrication Science, 1991, 3(1):51~72
Wei D P, Spikes H A. The lubricity of diesel fuels. Wear, 1986, 111, 217~235
William R, Ruhe J R. Reduced Color Molybdenum-Containing Composition and a Method of Making same. US, 0324949, 2003
Winer W O. Future trends in tribology. Wear, 1990, 136: 19~27
Zheng P Y, Han X A, Wang R L. The mechanism of friction reduction of sulfurized oxymolybdenum di-(2-ethylhexyl)-phosphorodithioate under boundary lubrication. ASLE preprint No. 86-TC-4E-1
陈波水.稀土化合物的润滑性能.中国稀土学报,1998,16(4): 358~360
陈耕.润滑剂与添加剂,北京:高等教育出版社,1993
范培文.威布尔概率纸在汽车零部件可靠性分析与评价工作中的应用,汽车科技,2002.4
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