CN110317229A - 一种酯类润滑油极压抗磨添加剂 - Google Patents
一种酯类润滑油极压抗磨添加剂 Download PDFInfo
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- C07D233/56—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms
- C07D233/58—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, not condensed with other rings having two double bonds between ring members or between ring members and non-ring members with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms, attached to ring nitrogen atoms
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- C07F9/02—Phosphorus compounds
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- C07F9/17—Esters of thiophosphoric acids with hydroxyalkyl compounds without further substituents on alkyl
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Abstract
本发明公开了一种不含金属元素的二烷基二硫代磷酸咪唑盐及其制备方法,作为酯类润滑油基础油的极压抗磨添加剂。第一步先合成了二辛基二硫代磷酸,然后将二辛基二硫代磷酸与1,3‑二辛基咪唑反应得目标产物。本发明公开的二烷基二硫代磷酸咪唑盐极压抗磨添加剂应用于己二酸二异辛酯、新戊基多元醇酯、癸二酸异辛酯等酯类润滑油基础油中。采用Optimol‑SRV IV摩擦磨损试验机、MicroXAM‑3D三维轮廓仪、GB/T12583润滑剂极压性能测定法(四球法)进行摩擦学性能评定,结果显示,本发明公开的极压抗磨添加剂具有优异的摩擦学性能。
Description
技术领域
本发明涉及一种二辛基二硫代磷酸咪唑盐作为酯类润滑油抗磨添加剂的制备及使用方法。
背景技术
润滑油基础油分为矿物型基础油和合成基础油。矿物型基础油是由原油加工提炼而成,主要是C20-C70烃类化合物。合成型基础油包括合成烃、聚醚、合成酯等。矿物油结构稳定,生物降解性差,会长期滞留在水和土壤中,造成污染环境。随着润滑油的广泛使用和对环境的日益关注,人们越来越重视润滑油对环境的污染问题,矿物型基础油使用越来越受到限制。合成酯类基础油是通过提炼动、植物脂肪酸和不同醇通过酯化、中和、过滤等工艺合成的单酯、双酯、多元醇酯等化合物。与石油基润滑油相比,合成酯类基础油具有较好的生物降解性,此外还具有较好的氧化安定性、低温流动性和润滑性等优点,是一类性能优异的润滑油基础油,已经应用于内燃机油、抗燃液压油、合成空压机油、齿轮油、轧制油、金属切削油、高温链条油等。因此,酯类基础油具有广泛的应用前景。
目前,最常用的抗磨剂是二烷基二硫代磷酸盐,是一类应用最广且综合性能较好的润滑油添加剂,它同时具有良好的抗氧化、抗腐蚀及抗磨作用、中等的极压性能和较好的热稳定性能。但是,由于其分子中含有金属离子,其实际应用受到了限制。
发明内容
本发明将合成一种不含金属元素的二烷基二硫代磷酸咪唑盐,并将其加入酯类润滑油中,提高酯类润滑油的极压抗磨性能。
本发明首先合成了二辛基二硫代磷酸,然后将二辛基二硫代磷酸和1,3-二辛基咪唑反应得目标产物,合成路线如图1所示。
具体合成方法如下:
向三口烧瓶加入一定量的五硫化二磷,慢慢滴加过量的正辛醇,固体完全溶解后,缓慢加热至60℃~100℃,反应至溶液澄清;减压蒸馏,取175℃~180℃馏分,为O,O-二辛基二硫代磷酸。
以氯仿作溶剂,将等物质的量的0,O-二辛基二硫代磷酸和1,3-二辛基咪唑溴盐混合,常温搅拌反应0.5~1小时,然后用蒸馏水洗至中性,除去生成的氢溴酸,分出有机层,除去溶剂,得到浅黄色粘稠液体产物,为目标产物。
润滑性能评价
将目标产物加入酯类油中,采用Optimol-SRV IV摩擦磨损试验机评价润滑剂的摩擦学性能,摩擦系数由计算机给出;采用MicroXAM-3D三维轮廓仪观察磨斑的表面形貌并计算出磨损体积。试验条件为:载荷294N、频率25Hz、振幅1mm,试验时间30min,温度为室温。上试球和下试盘均为GCr15钢(SAE52100,硬度为59~61HRC),上试球直径为10mm;下试盘直径为24mm,厚度为8.0mm。每次试验前在球盘接触部位滴加两滴润滑剂。
极压性能按GB/T12583润滑剂极压性能测定法(四球法)进行评定,采用济南试验机厂生产的MRS-1J型四球试验机,所用钢球为GCr15标准钢球(AISI-52100),直径为12.7mm,硬度为59~61HRC。
将O,O-二辛基二硫代磷酸咪唑盐加入己二酸二异辛酯基础油中,质量分数为0.5%、 01.0%和2.0%。摩擦学性能测试结果显示,随着质量浓度的增加,摩擦系数和磨损体积逐渐减小。当质量浓度为0.5%时,摩擦系数从0.85左右减少至0.55左右,磨损体积从84.2×10-5mm3减少至50×10-5mm3左右;当浓度为2.0%时,摩擦系数减少至0.34,磨损体积减少至 20.6×10-5mm3。
按GB/T12583润滑剂极压性能测定法(四球法)进行评定了抗磨剂对酯类基础油极压性能的影响。结果表明,随着极压抗磨剂的增加,PB值增加,当浓度为2.0%时,极压值从基础油的392N增加至981N,说明产品具有较好的极压性能。
附图说明
图1为硫代磷酸咪唑盐的合成路线图。
具体实施方式:
实施例一:
向三口烧瓶加入0.20mol的五硫化二磷,慢慢滴加0.45mol正辛醇,固体完全溶解后,缓慢加热至80℃,反应至溶液澄清;减压蒸馏,取175℃~180℃馏分,为O,O-二辛基二硫代磷酸。
以氯仿作溶剂,将0.10mol的O,O-二辛基二硫代磷酸和0.10mol的1,3-二辛基咪唑溴盐混合,常温搅拌反应0.5小时,然后用蒸馏水洗至中性,除去生成的氢溴酸,分出有机层,除去溶剂,得到浅黄色粘稠液体产物,为目标产物二辛基二硫代磷酸咪唑盐极压抗磨剂。
将二辛基二硫代磷酸咪唑盐极压抗磨剂加入己二酸二异辛酯基础油中,质量百分含量为1.0%。摩擦系数从0.85左右减少至0.46左右,磨损体积从84.2×10-5mm3减少至60.0×10-5mm3左右。
实施例二:
将实施例一中合成的二辛基二硫代磷酸咪唑盐极压抗磨剂加入新戊基多元醇酯基础油中,质量百分含量为2.0%。摩擦系数从0.80左右减少至0.41左右,磨损体积从76.6×10-5mm3减少至55.0×10-5mm3左右。
实施例三:
将实施例一中合成的二辛基二硫代磷酸咪唑盐极压抗磨剂加入癸二酸异辛酯基础油中,质量百分含量为2.0%。摩擦系数从0.79左右减少至0.38左右,磨损体积从79.3×10-5mm3减少至54.0×10-5mm3左右。
Claims (3)
1.一种酯类润滑油极压抗磨添加剂,其特征在于所述极压抗磨剂的化学结构式为:
2.如权利要求1所述的一种酯类润滑油极压抗磨添加剂,其特征在于应用于酯类润滑油基础油中;
3.如权利要求1所述的一种酯类润滑油极压抗磨添加剂,其特征在于加入质量浓度为0.5%~4.0%。
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张森田等: ""硫代磷酸酯的合成及其缓蚀性能的研究"", 《石油化工》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114015422A (zh) * | 2021-10-26 | 2022-02-08 | 中石化南京化工研究院有限公司 | 一种环保型钻井液高性能润滑剂 |
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