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CN1058985C - Nano size rare earth fluoride lubricant oil additive - Google Patents

Nano size rare earth fluoride lubricant oil additive Download PDF

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Publication number
CN1058985C
CN1058985C CN98123519A CN98123519A CN1058985C CN 1058985 C CN1058985 C CN 1058985C CN 98123519 A CN98123519 A CN 98123519A CN 98123519 A CN98123519 A CN 98123519A CN 1058985 C CN1058985 C CN 1058985C
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rare earth
water
lubricating oil
nano
fluorinated
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CN1218104A (en
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张泽抚
刘维民
薛群基
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Qingdao Delong Special Lubricating Oil Co Ltd
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种纳米氟化稀土润滑油添加剂及其制备方法。本发明由水溶性稀土无机盐、分散剂、表面活性剂、促进剂、基础油、氟化钠组成。本发明的纳米氟化稀土颗粒尺寸在10~50纳米,成功地解决了氟化稀土在润滑油中的分散问题,它是性能优良的润滑油极压、抗磨添加剂。The invention discloses a nanometer fluorinated rare earth lubricating oil additive and a preparation method thereof. The invention consists of water-soluble rare earth inorganic salt, dispersant, surface active agent, accelerator, base oil and sodium fluoride. The particle size of the nanometer rare earth fluoride is 10-50 nanometers, which successfully solves the dispersion problem of the rare earth fluoride in lubricating oil, and is an excellent extreme pressure and anti-wear additive for lubricating oil.

Description

纳米氟化稀土润滑油添加剂Nano Fluorinated Rare Earth Lubricating Oil Additives

本发明公开了一种纳米氟化稀土润滑油添加剂及其制备方法。The invention discloses a nanometer fluorinated rare earth lubricating oil additive and a preparation method thereof.

稀土氟化物在润滑脂中得到了广泛应用,U.S.4,507,214,4,946,607,4,946,608公开了氟化稀土在润滑油脂中具有良好的润滑性。在CN 1,032549A,1,032,550A中,稀土氟化物已被成功的应用于铁路润滑成膜膏中,并取得了非常好的润滑效果。由于其在润滑油中的分散性很差,从而限制了其在润滑油中的广泛应用。Rare earth fluorides have been widely used in lubricating greases. U.S. 4,507,214, 4,946,607, and 4,946,608 disclose that rare earth fluorides have good lubricity in lubricating greases. In CN 1,032549A, 1,032,550A, rare earth fluorides have been successfully applied in railway lubricating film-forming pastes, and have achieved very good lubricating effects. Due to its poor dispersibility in lubricating oil, its wide application in lubricating oil is limited.

本发明的目的在于提供一种润滑油添加剂及其制备方法,它在润滑油中具有良好的分散性、极压和抗磨性能。The object of the present invention is to provide a lubricating oil additive and its preparation method, which has good dispersibility, extreme pressure and anti-wear properties in lubricating oil.

本发明由水溶性稀土无机盐、分散剂、表面活性剂、促进剂、基础油、氟化钠组成。The invention consists of water-soluble rare earth inorganic salt, dispersant, surface active agent, accelerator, base oil and sodium fluoride.

纳米氟化稀土润滑油添加剂由:水溶性稀土无机盐10~20、分散剂10~30、表面活性剂0.1~5、促进剂10~30、基础油40~60、氟化钠2~5(重量百分含量)组成。Nano fluorinated rare earth lubricating oil additives are composed of: water-soluble rare earth inorganic salt 10-20, dispersant 10-30, surfactant 0.1-5, accelerator 10-30, base oil 40-60, sodium fluoride 2-5 ( weight percent) composition.

稀土无机盐为氯化稀土、硝酸稀土或高氯酸稀土,稀土为镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥中的一种或几种。The rare earth inorganic salt is rare earth chloride, rare earth nitrate or rare earth perchlorate, and the rare earth is one or more Several kinds.

分散剂为聚异丁烯单丁二酰亚胺、聚异丁烯双丁二酰亚胺、石油磺酸钙、石油磺酸镁中的一种或几种。The dispersant is one or more of polyisobutylene monosuccinimide, polyisobutylene bis-succinimide, calcium petroleum sulfonate, and magnesium petroleum sulfonate.

表面活性剂为司本-20、司本-80、吐温-40、吐温-60的一种或几种。Surfactant is one or more of Siben-20, Siben-80, Tween-40 and Tween-60.

促进剂为水、甲醇、乙醇、丙醇、丁醇、戊醇、己醇、辛醇的一种或几种的混合物。The accelerator is one or a mixture of water, methanol, ethanol, propanol, butanol, pentanol, hexanol, and octanol.

基础油为中性石蜡基精制基础油(40℃粘度为28.8-35.2mm2/s)。The base oil is a neutral paraffin-based refined base oil (viscosity of 28.8-35.2 mm 2 /s at 40°C).

其制备方法如下:Its preparation method is as follows:

将水溶性无机稀土盐10~20wt.%溶于水中,将分散剂10~30wt.%、表面活性剂0.1~5wt.%、促进剂10~30wt.%、中性石蜡基精制基础油(40℃粘度为28.8-35.2mm2/s)40~60wt.%,将苯0.6份(以上述总量为1份)与上述溶液混合,在水浴中搅拌半小时,缓慢滴加2~5wt.%氟化钠的水溶液,在水浴中搅拌5~10小时。减压蒸除苯、水等物质。10-20wt.% of water-soluble inorganic rare earth salt is dissolved in water, 10-30wt.% of dispersant, 0.1-5wt.% of surfactant, 10-30wt.% of accelerator, neutral paraffin-based refined base oil (40 ℃ viscosity is 28.8-35.2mm 2 /s) 40 ~ 60wt.%, 0.6 parts of benzene (1 part based on the above total amount) is mixed with the above solution, stirred in a water bath for half an hour, slowly drop 2 ~ 5wt.% The aqueous solution of sodium fluoride was stirred in a water bath for 5-10 hours. Substances such as benzene and water were evaporated under reduced pressure.

本发明所合成的含氮有机物修饰的纳米氟化稀土是一类非常有效的润滑油极压、抗磨添加剂。其作为润滑油添加剂的添加量为0.1wt%~8wt%。The nanometer rare earth fluoride synthesized by nitrogen-containing organic matter modified by the invention is a kind of very effective extreme pressure and anti-wear additives for lubricating oil. Its addition amount as lubricating oil additive is 0.1wt%-8wt%.

为了更好地理解本发明,通过实例进行说明。In order to better understand the present invention, it is illustrated by examples.

实例1将1.86g氯化镧溶于水中,再将2g聚异丁烯单丁二酰亚胺、0.2g石油磺酸钙0.3g司本-80、7g基础油与上述溶液混合,加入10ml苯,在水浴中搅拌半小时,缓慢滴加1.1g氟化钠的水溶液,在水浴中搅拌7小时。加入50ml的苯以便过滤。将滤液减压蒸除苯、水等挥发性物质。Example 1 Dissolve 1.86g lanthanum chloride in water, then mix 2g polyisobutylene monosuccinimide, 0.2g petroleum calcium sulfonate, 0.3g Siben-80, and 7g base oil with the above solution, add 10ml benzene, and Stir in a water bath for half an hour, slowly add 1.1 g of an aqueous solution of sodium fluoride dropwise, and stir in a water bath for 7 hours. Add 50ml of benzene for filtration. The filtrate was evaporated under reduced pressure to remove volatile substances such as benzene and water.

实例2将2.22g硝酸钐溶于水中,再将3g聚异丁烯双丁二酰亚胺、0.1g石油磺酸钙、0.3g司本-80、10ml甲醇、7g基础油与上述溶液混合,加入14ml苯,在水浴中搅拌半小时,缓慢滴加1.1g氟化钠溶液,在水浴中搅拌9小时。加入50ml的苯以便过滤。将滤液减压蒸除苯、水等挥发性物质。Example 2 Dissolve 2.22g of samarium nitrate in water, then mix 3g of polyisobutylene bis-succinimide, 0.1g of calcium petroleum sulfonate, 0.3g of Siben-80, 10ml of methanol, and 7g of base oil with the above solution, and add 14ml Benzene, stirred in a water bath for half an hour, slowly added dropwise 1.1 g of sodium fluoride solution, and stirred in a water bath for 9 hours. Add 50ml of benzene for filtration. The filtrate was evaporated under reduced pressure to remove volatile substances such as benzene and water.

实例3将2.35g高氯酸铒溶于水中,再将2.1g聚异丁烯双丁二酰亚胺、0.2g石油磺酸镁、0.3g司本-80、6g基础油与上述溶液混合,加入15ml苯,在水浴中搅拌半小时,缓慢滴加1.7g氟化钠的水溶液,在水浴中搅拌8小时。加入50ml的苯以便过滤。将滤液减压蒸除苯、水等挥发性物质。Example 3 Dissolve 2.35g erbium perchlorate in water, then mix 2.1g polyisobutylene bis-succinimide, 0.2g magnesium petroleum sulfonate, 0.3g Siben-80, 6g base oil with the above solution, add 15ml Benzene, stirred in a water bath for half an hour, slowly added dropwise an aqueous solution of 1.7 g of sodium fluoride, and stirred in a water bath for 8 hours. Add 50ml of benzene for filtration. The filtrate was evaporated under reduced pressure to remove volatile substances such as benzene and water.

实例4反应条件同实例1,将氯化镧中的镧分别替换为铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥,可得到相应的纳米氟化稀土。The reaction conditions of Example 4 are the same as in Example 1, and the lanthanum in lanthanum chloride is replaced by cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium respectively to obtain the corresponding nanometer fluorine rare earths.

对实例1中所制备的纳米氟化镧在液体石蜡中的最大无卡咬负荷和抗磨性能用四球摩擦磨损试验机进行评价。为了便于对比,对二烷基二硫代磷酸锌(ZDDP)在液体石蜡中的最大无卡咬负荷和抗磨性也进行了测量。抗磨实验的操作条件为:负荷392N,实验时间30min,转速1450rpm。实验结束后,测量钢球的磨斑直径(WSD),结果列于表1中。The maximum non-seize load and anti-wear performance of the nano-lanthanum fluoride prepared in Example 1 in liquid paraffin were evaluated with a four-ball friction and wear tester. For comparison, the maximum no-seize load and wear resistance of zinc dialkyldithiophosphate (ZDDP) in liquid paraffin were also measured. The operating conditions of the anti-wear test are: load 392N, test time 30min, rotational speed 1450rpm. After the experiment, the wear spot diameter (WSD) of the steel ball was measured, and the results are listed in Table 1.

由上述实验结果可以看出,此类纳米氟化稀土作为润滑油添加剂具有良好的极压性能和抗磨损性能,是一类具有广泛应用前景的润滑油极压、抗磨添加剂。表1最大无卡咬负荷(PB值)和抗磨性能评价结果添加剂    浓度(wt%)  PB值(N)   WSD(mm)液体石蜡    100        372        0.72It can be seen from the above experimental results that this kind of nano-rare earth fluoride has good extreme pressure performance and anti-wear performance as a lubricating oil additive, and is a kind of extreme pressure and anti-wear additive for lubricating oil with wide application prospects. Table 1 Maximum non-seize load (P B value) and anti-wear performance evaluation results Additive concentration (wt%) P B value (N) WSD (mm) liquid paraffin 100 372 0.72

        0.5        686        0.44本发明0.5 686 0.44 Invention

        1          735        0.421 735 0.42

        2          764        0.442 764 0.44

        3          764        0.62ZDDP        1          784        0.503 764 0.62ZDDP 1 784 0.50

Claims (6)

1、一种纳米氟化稀土润滑油添加剂由:水溶性稀土无机盐     10~20分散剂              10~30司本-80             0.1~5促进剂              10~30基础油              40~60氟化钠              2~5重量百分含量组成。1. A nanometer fluorinated rare earth lubricating oil additive is composed of: water-soluble rare earth inorganic salt 10-20 dispersant 10-30 Siben-80 0.1-5 accelerator 10-30 base oil 2-60 weight of sodium fluoride percentage composition. 2、如权利要求1所述纳米氟化稀土润滑油添加剂,其特征在于水溶性稀土无机盐为氯化稀土、硝酸稀土或高氯酸稀土,稀土为镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥的一种。2. Nano-fluorinated rare earth lubricating oil additive as claimed in claim 1, characterized in that the water-soluble rare earth inorganic salt is rare earth chloride, rare earth nitrate or rare earth perchlorate, and the rare earth is lanthanum, cerium, praseodymium, neodymium, samarium, europium , Gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium. 3、如权利要求1所述纳米氟化稀土润滑油添加剂,其特征在于分散剂为聚异丁烯单丁二酰亚胺、聚异丁烯双丁二酰亚胺、石油磺酸钙、石油磺酸镁的一种。3. Nano-fluorinated rare earth lubricating oil additive as claimed in claim 1, characterized in that the dispersant is polyisobutylene monosuccinimide, polyisobutylene bis-succinimide, calcium petroleum sulfonate, magnesium petroleum sulfonate A sort of. 4、如权利要求1所述纳米氟化稀土润滑油添加剂,其特征在于促进剂为水、甲醇、乙醇、丙醇、丁醇的一种。4. The nano-fluorinated rare earth lubricating oil additive according to claim 1, wherein the accelerator is one of water, methanol, ethanol, propanol, and butanol. 5、如权利要求1所述纳米氟化稀土润滑油添加剂,其特征在于基础油为中性石蜡基精制矿物油,40℃的运动粘度为28.8-35.2mm2/s。5. The nano-fluorinated rare earth lubricating oil additive according to claim 1, characterized in that the base oil is neutral paraffin-based refined mineral oil, and the kinematic viscosity at 40°C is 28.8-35.2 mm 2 /s. 6、如权利要求1所述纳米氟化稀土润滑油添加剂的制备方法包括:将水溶性无机稀土盐10~20wt.%溶于水中,将分散剂10~30wt.%、表面活性剂0.1~5wt.%、促进剂10~30wt.%、中性石蜡基精制基础油40~60wt.%,其40℃粘度为28.8-35.2mm2/s,以上述总量为1份,再将苯0.6份与上述溶液混合,在水浴中搅拌半小时,缓慢滴加2~5wt.%氟化钠的水溶液,在水浴中搅拌5~10小时,减压蒸除苯、水物质。6. The preparation method of nano-fluorinated rare earth lubricating oil additives as claimed in claim 1 comprises: dissolving 10-20wt.% of water-soluble inorganic rare-earth salt in water, adding 10-30wt.% of dispersant and 0.1-5wt.% of surfactant .%, accelerator 10-30wt.%, neutral paraffin-based refined base oil 40-60wt .%. Mix with the above solution, stir in a water bath for half an hour, slowly add 2 to 5 wt.% sodium fluoride aqueous solution dropwise, stir in a water bath for 5 to 10 hours, evaporate benzene and water under reduced pressure.
CN98123519A 1998-10-08 1998-10-08 Nano size rare earth fluoride lubricant oil additive Expired - Fee Related CN1058985C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6316377B1 (en) * 1999-09-10 2001-11-13 Battelle Memorial Institute Rare earth oxide fluoride nanoparticles and hydrothermal method for forming nanoparticles
CN100338200C (en) * 2004-04-14 2007-09-19 中国石油化工股份有限公司 Process for preparing lubricating oil additive containing nano microparticles
CN100395320C (en) * 2006-03-15 2008-06-18 华东理工大学 Fluorine-containing rare earth nano lubricating oil additive and preparation method thereof
CN100494330C (en) * 2007-05-16 2009-06-03 龚; Nano bionic self-organization lubricating oil additive and preparation method thereof
CN103540388B (en) * 2013-10-24 2014-12-31 大连海事大学 A kind of FD bearing oil composition, its preparation method and application
CN107151571A (en) * 2017-06-05 2017-09-12 合肥嘉仕诚能源科技有限公司 A kind of biomass fuel and preparation method
CN108410539B (en) * 2018-03-01 2021-04-27 清华大学天津高端装备研究院 Oil-soluble nano rare earth anti-wear lubricating oil additive and preparation method thereof
CN110205185A (en) * 2019-06-11 2019-09-06 日生能科技(厦门)有限公司 A kind of rare earth compound lube oil additive manufacturing method
CN111548842A (en) * 2020-05-21 2020-08-18 成都玉龙化工有限公司 Lubricant and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4946607A (en) * 1988-10-10 1990-08-07 Rhone-Poulenc Chimie Aqueous lubricant dispersions of rare earth halides
CN1180079A (en) * 1995-07-06 1998-04-29 中国科学院兰州化学物理研究所 Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method
CN1183461A (en) * 1995-07-06 1998-06-03 中国科学院兰州化学物理研究所 Sulfo-organo-compound modified dichalcogenide nm micropowder and preparing method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4946607A (en) * 1988-10-10 1990-08-07 Rhone-Poulenc Chimie Aqueous lubricant dispersions of rare earth halides
CN1180079A (en) * 1995-07-06 1998-04-29 中国科学院兰州化学物理研究所 Fatty acid modifying metallic oxide or hydroxide nanometre powder and its preparing method
CN1183461A (en) * 1995-07-06 1998-06-03 中国科学院兰州化学物理研究所 Sulfo-organo-compound modified dichalcogenide nm micropowder and preparing method thereof

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