CN117568087B - 一种长寿命汽车无极变速器油及其制备方法 - Google Patents
一种长寿命汽车无极变速器油及其制备方法 Download PDFInfo
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- C07D285/00—Heterocyclic compounds containing rings having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by groups C07D275/00 - C07D283/00
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- C10M2205/0285—Organic macromolecular hydrocarbon compounds or fractions, whether or not modified by oxidation as ingredients in lubricant compositions containing acyclic monomers containing aliphatic monomers having more than four carbon atoms used as base material
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Abstract
本发明属于润滑油技术领域，具体涉及一种长寿命汽车无极变速器油及其制备方法，包括以下步骤：将二油酸新戊二醇酯、壬二酸二(2‑乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油混合均匀，加入清净分散剂、抗氧剂、防锈剂、抗磨剂、摩擦改进剂、金属减活剂、抗泡剂，加入粘度指数改进剂，混匀后冷却，即得；所述金属减活剂为噻二唑衍生物，其结构中含有烷基长链、酯基与二硫键，油溶性、极压抗磨性能优异，同时还可抑制金属的腐蚀，与其他原料协同增效，有效改善了油品的使用性能。本发明提供的无极变速器油具有优异的抗磨减摩性、防锈性、抗氧化性、闪点和倾点，同时还具有较高的牵引系数和粘度指数，油品的使用寿命可达到15‑20万公里。
Description
技术领域
本发明属于润滑油技术领域，具体涉及一种长寿命汽车无极变速器油及其制备方法。
背景技术
润滑油在无级变速器传动系统中除了发挥润滑冷却的作用外，还要具备合适的动静摩擦因数以及减磨的功效，从而满足传动系统高效长寿命的使用要求，是系统运行不可缺少的材料。随着无级变速器的应用越来越广泛，其传动形式对润滑油的性能要求越来越高，无级变速器传动液（无级变速器油）对于无级变速器的传动效率和寿命有很大的影响。
申请号为CN201310542866.0的专利提供了一种汽车无级变速器传动油，包括以下组分：Ⅲ类基础油、抗磨剂、粘度指数改进剂、降凝剂、碱土金属清净剂、分散剂、抗氧剂、摩擦改进剂和抗泡剂，该发明将Ⅲ类基础油与其他添加剂优化配伍，得到的无级变速器传动油具有良好的粘度指数、氧化安定性、剪切安定性、抗磨性、低温性能，还具有大扭矩、高牵引系数、高传动效率，但该无极变速器油使用寿命一般在6万公里，且其会导致汽车无极变速器操作舒适感下降，噪音大；申请号为CN201811201860.6的专利提供了一种氧化石墨烯润滑添加剂，并将其应用于自动变速箱油中，很好地改善了自动变速箱油的防锈性、抗氧化性、极压抗磨性能与摩擦特性，氧化石墨烯主要起减摩抗磨作用，应用于固体润滑和低速大负荷设备时能发挥出较好的效果，当发动机转数超过1000r/min时，其作用较小，此外，氧化石墨烯作为固体悬浮剂，在一定的时间及温度条件下会发生析出现象，其析出物会造成油路的堵塞，并加速油泥的形成，减少油品使用寿命。为满足市场需求，迫切需要开发一种综合性能优异、使用寿命长的无级变速器油。
发明内容
针对现有技术的不足，本发明的目的在于提供一种长寿命汽车无极变速器油,该无极变速器油具有优异的抗磨减摩性、防锈性、抗氧化性、闪点和倾点，同时还具有较高的牵引系数和粘度指数，满足了现代汽车无极变速器润滑保护的要求；本发明还提供了该无极变速器油的制备方法。
本发明为实现上述目的所采取的技术方案为：
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯15-25份、壬二酸二(2-乙基己基)酯25-35份、季戊四醇油酸酯5-15份、聚α烯烃基础油35-45份、粘度指数改进剂4-10份、抗氧剂0.5-1.5份、清净分散剂1-5份、金属减活剂0.2-0.5份、防锈剂0.3-1.0份、抗磨剂1-3份、摩擦改进剂1-4份、抗泡剂0.01-0.05份，所述金属减活剂为噻二唑衍生物，噻二唑衍生物的制备方法如下：
S1、将3,3'-二硫代二丙酸分散于2-甲基四氢呋喃中，依次加入乙酸铬、1,2-环氧丁烷，升温至55-65℃，搅拌反应6-11h，过滤，取滤液，经减压蒸馏、干燥，得到中间体；
S2、将步骤S1所得中间体分散于2-甲基四氢呋喃中，依次加入对甲苯磺酸、1,2,3-噻二唑-4-羧酸，升温至70-80℃，搅拌反应5-8h，过滤，取滤液，经减压蒸馏、萃取、浓缩、干燥，得到噻二唑衍生物；
噻二唑衍生物的合成路线如下：
;
。
本发明以3,3'-二硫代二丙酸、1,2-环氧丁烷为起始原料，在乙酸铬催化作用下，发生环氧化合物开环反应，得到中间体；中间体结构中含有羟基，在对甲苯磺酸作用下与1,2,3-噻二唑-4-羧酸结构中的羧基发生酯化反应，得到噻二唑衍生物。
为了得到噻二唑衍生物，并保证产物一致性，步骤S1中所述3,3'-二硫代二丙酸、乙酸铬、1,2-环氧丁烷的摩尔比为1:0.02-0.03:1.6-2.2，2-甲基四氢呋喃中3,3'-二硫代二丙酸的加入量为0.15-0.28g/mL；步骤S2中所述中间体、对甲苯磺酸、1,2,3-噻二唑-4-羧酸的摩尔比为1:0.025-0.033:1.7-2.4，2-甲基四氢呋喃中中间体的加入量为0.20-0.25g/mL。
优选地，所述粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯、聚乙烯基正丁醚和苯乙烯-马来酸酐共聚物中的一种或两种以上；所述抗氧剂为4,4'-二辛基二苯胺或2,4-二甲基-6-叔丁基苯酚；所述清净分散剂为硼化聚异丁烯基丁二酰亚胺；所述防锈剂为十二烯基丁二酸；所述抗磨剂为硫代磷酸三苯酯、亚磷酸二正丁酯、磷酸三甲酚酯中的一种或两种以上；所述摩擦改进剂为油酸乙二醇酯、正十六烷胺和油酸酰胺中的一种或两种以上；所述抗泡剂为二甲基硅油、乙基硅油、丙烯酸辛酯中的一种或两种以上。
本发明通过两步法合成噻二唑衍生物，其具有极好的油溶性能，可以在润滑油中作为金属减活剂，还具有很好的极压抗磨特性。本发明以二油酸新戊二醇酯、壬二酸二(2-乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油为原料制备混合煤制基础油，其具有较高的粘度指数，保证了混合煤制基础油在高温下的油膜厚度。所述抗磨剂选用无灰型硫代磷酸三苯酯，其具有良好的油溶性、减摩和抗磨性，与金属减活剂复配使用，能够极大地提高油品的防腐蚀性能。发动机设备中的各种金属材质，如铜、铁等均会起催化作用加速油品的氧化变质，会导致润滑油粘度增加，生成酸性物质腐蚀金属材质，生成各种炭状或沥青状沉淀物质如漆膜等堵塞管路，以上变化均对油品的继续使用和设备正常运行带来不利影响，本发明将硫代磷酸三苯酯、4,4'-二辛基二苯胺与噻二唑衍生物复配使用，显著提高油品的抗氧和抗腐性能，减少油泥生成，保证油品品质，延长油品使用寿命。
本发明还提供了一种长寿命汽车无极变速器油的制备方法，包括以下步骤：将二油酸新戊二醇酯、壬二酸二(2-乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油混合均匀，升温至50-60℃，依次加入清净分散剂、抗氧剂、防锈剂、抗磨剂、摩擦改进剂、金属减活剂、抗泡剂，搅拌20-40min，最后加入粘度指数改进剂，继续搅拌40-60min，冷却至室温，即得。
本发明具有如下有益效果：
（1）本发明通过两步法在噻二唑分子结构中引入烷基长链、酯基与二硫键，得到噻二唑衍生物。该噻二唑衍生物具有优异的油溶性、极压抗磨性；作为噻二唑多硫化物，还能捕捉油品中的活性硫，抑制金属的腐蚀，二硫键可在金属表面形成硫化膜，从而有效地抑制了金属离子对油品的催化作用，改善油品的使用性能；此外，噻二唑衍生物还可作为辅助抗氧化剂，与硫代磷酸三苯酯、4,4'-二辛基二苯胺协同增效，进一步提高油品的抗氧和抗腐性能。
（2）本发明提供的噻二唑衍生物与混合煤制基础油及其它添加剂有良好的相容性、配伍性，各组分优化配比，协同增效，显著提高了油品的综合性能。本发明提供的无极变速器油具有优异的抗磨减摩性、防锈性、抗氧化性、闪点和倾点，同时还具有较高的牵引系数和粘度指数，油品的使用寿命可达到15-20万公里；此外，酯类全合成配方具有一定的生物降解性，能减少对环境的污染，适合大范围地推广和应用。
具体实施方式
下面将结合本申请实施例，对本申请实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本申请一部分实施例，而不是全部的实施例。基于本申请中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本申请保护的范围。
二油酸新戊二醇酯，40℃运动粘度28-32mm2/s，购自山东信发瑞捷新材料科技有限公司；季戊四醇油酸酯，型号PETO，运动粘度68.3mm2/s，购自济南永宸化工有限公司；壬二酸二(2-乙基己基)酯，货号00018，购自湖北玖丰隆化工有限公司；聚α烯烃基础油，品牌英力士INEOS，型号聚α烯烃PAO Durasyn® 164，购自上海棋成润滑材料有限公司；聚异丁烯，25℃密度0.92g/cm3，有效成分含量99%，购自锦州精联润滑油添加剂有限公司；聚甲基丙烯酸酯，型号TC-602HB，购自石家庄市藁城区天成油品添加剂厂；硫代磷酸三苯酯，型号T309，磷含量≥8.9%，硫含量≥9.3%，硼化聚异丁烯基丁二酰亚胺，品牌GDR，型号BT154，均购自锦州加多润材料科技有限公司；油酸乙二醇酯，型号T403B，购自河北拓驰润滑油销售有限公司；二甲基硅油，有效含量99%，购自济南硅港化工有限公司；十二烯基丁二酸，型号T746，购自新乡市金博润滑新材料有限公司。下述实施例中所用原料均为普通市售产品。
实施例1
一种噻二唑衍生物的制备方法，包括以下步骤：
S1、将3,3'-二硫代二丙酸分散于2-甲基四氢呋喃中，依次加入乙酸铬、1,2-环氧丁烷，升温至60℃，搅拌反应8h，过滤，取滤液，减压蒸馏除去2-甲基四氢呋喃，于50℃真空干燥12h，得到中间体，其中3,3'-二硫代二丙酸、乙酸铬、1,2-环氧丁烷的摩尔比为1:0.024:1.8，2-甲基四氢呋喃中3,3'-二硫代二丙酸的加入量为0.2g/mL；
S2、将步骤S1所得中间体分散于2-甲基四氢呋喃中，依次加入对甲苯磺酸、1,2,3-噻二唑-4-羧酸，升温至75℃，搅拌反应6h，过滤，取滤液，减压蒸馏除去2-甲基四氢呋喃，加入乙酸乙酯和水进行萃取，取有机相浓缩，于60℃真空干燥24h，得到噻二唑衍生物，其中乙酸乙酯与水的体积比为1:1，中间体、对甲苯磺酸、1,2,3-噻二唑-4-羧酸的摩尔比为1:0.028:2.1，2-甲基四氢呋喃中中间体的加入量为0.22g/mL；
噻二唑衍生物的核磁结果为：1H NMR(300MHz，DMSO-d6) δ 8.19（s，2H），5.14-5.18（m，2H），4.57-4.61（m，2H），4.34-4.38（m，2H），2.95（t，4H），2.51（t，4H），1.70-1.77（m，4H），0.89（t，6H）。
实施例2
一种噻二唑衍生物的制备方法，包括以下步骤：
S1、将3,3'-二硫代二丙酸分散于2-甲基四氢呋喃中，依次加入乙酸铬、1,2-环氧丁烷，升温至55℃，搅拌反应11h，过滤，取滤液，减压蒸馏除去2-甲基四氢呋喃，于50℃真空干燥12h，得到中间体，其中3,3'-二硫代二丙酸、乙酸铬、1,2-环氧丁烷的摩尔比为1:0.02:1.6，2-甲基四氢呋喃中3,3'-二硫代二丙酸的加入量为0.15g/mL；
S2、将步骤S1所得中间体分散于2-甲基四氢呋喃中，依次加入对甲苯磺酸、1,2,3-噻二唑-4-羧酸，升温至70℃，搅拌反应5h，过滤，取滤液，减压蒸馏除去2-甲基四氢呋喃，加入乙酸乙酯和水进行萃取，取有机相浓缩，于60℃真空干燥24h，得到噻二唑衍生物，其中乙酸乙酯与水的体积比为1:1，中间体、对甲苯磺酸、1,2,3-噻二唑-4-羧酸的摩尔比为1:0.025:1.7，2-甲基四氢呋喃中中间体的加入量为0.2g/mL。
实施例3
一种噻二唑衍生物的制备方法，包括以下步骤：
S1、将3,3'-二硫代二丙酸分散于2-甲基四氢呋喃中，依次加入乙酸铬、1,2-环氧丁烷，升温至65℃，搅拌反应6h，过滤，取滤液，减压蒸馏除去2-甲基四氢呋喃，于50℃真空干燥12h，得到中间体，其中3,3'-二硫代二丙酸、乙酸铬、1,2-环氧丁烷的摩尔比为1:0.03:2.2，2-甲基四氢呋喃中3,3'-二硫代二丙酸的加入量为0.28g/mL；
S2、将步骤S1所得中间体分散于2-甲基四氢呋喃中，依次加入对甲苯磺酸、1,2,3-噻二唑-4-羧酸，升温至80℃，搅拌反应8h，过滤，取滤液，减压蒸馏除去2-甲基四氢呋喃，加入乙酸乙酯和水进行萃取，取有机相浓缩，于60℃真空干燥24h，得到噻二唑衍生物，其中乙酸乙酯与水的体积比为1:1，中间体、对甲苯磺酸、1,2,3-噻二唑-4-羧酸的摩尔比为1:0.033:2.4，2-甲基四氢呋喃中中间体的加入量为0.25g/mL。
实施例4
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯20份、壬二酸二(2-乙基己基)酯30份、季戊四醇油酸酯10份、聚α烯烃基础油40份、粘度指数改进剂6份、抗氧剂1份、清净分散剂3份、金属减活剂0.4份、防锈剂0.7份、抗磨剂2份、摩擦改进剂2份、抗泡剂0.03份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为实施例1所制备的噻二唑衍生物，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油。
一种长寿命汽车无极变速器油的制备方法，包括以下步骤：
将二油酸新戊二醇酯、壬二酸二(2-乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油在400r/min转速下搅拌混合均匀，升温至55℃，依次加入清净分散剂、抗氧剂、防锈剂、抗磨剂、摩擦改进剂、金属减活剂、抗泡剂，继续搅拌30min，最后加入粘度指数改进剂，继续搅拌50min，冷却至室温，即得。
实施例5
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯20份、壬二酸二(2-乙基己基)酯30份、季戊四醇油酸酯10份、聚α烯烃基础油40份、粘度指数改进剂6份、抗氧剂1份、清净分散剂3份、金属减活剂0.2份、防锈剂0.7份、抗磨剂2份、摩擦改进剂2份、抗泡剂0.03份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为实施例1所制备的噻二唑衍生物，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油；与实施例4的区别在于：改变了金属减活剂的重量份数。
实施例6
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯20份、壬二酸二(2-乙基己基)酯30份、季戊四醇油酸酯10份、聚α烯烃基础油40份、粘度指数改进剂6份、抗氧剂1份、清净分散剂3份、金属减活剂0.5份、防锈剂0.7份、抗磨剂2份、摩擦改进剂2份、抗泡剂0.03份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为实施例1所制备的噻二唑衍生物，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油；与实施例4的区别在于：改变了金属减活剂的重量份数。
实施例5-6所述长寿命汽车无极变速器油均按照实施例4所述方法制备。
实施例7
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯15份、壬二酸二(2-乙基己基)酯35份、季戊四醇油酸酯5份、聚α烯烃基础油45份、粘度指数改进剂4份、抗氧剂0.5份、清净分散剂1份、金属减活剂0.5份、防锈剂0.3份、抗磨剂3份、摩擦改进剂1份、抗泡剂0.01份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为实施例1所制备的噻二唑衍生物，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油。
一种长寿命汽车无极变速器油的制备方法，包括以下步骤：
将二油酸新戊二醇酯、壬二酸二(2-乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油在400r/min转速下搅拌混合均匀，升温至50℃，依次加入清净分散剂、抗氧剂、防锈剂、抗磨剂、摩擦改进剂、金属减活剂、抗泡剂，继续搅拌40min，最后加入粘度指数改进剂，继续搅拌60min，冷却至室温，即得。
实施例8
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯25份、壬二酸二(2-乙基己基)酯25份、季戊四醇油酸酯15份、聚α烯烃基础油35份、粘度指数改进剂10份、抗氧剂1.5份、清净分散剂5份、金属减活剂0.5份、防锈剂1份、抗磨剂1份、摩擦改进剂4份、抗泡剂0.05份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为实施例1所制备的噻二唑衍生物，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油。
一种长寿命汽车无极变速器油的制备方法，包括以下步骤：
将二油酸新戊二醇酯、壬二酸二(2-乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油在400r/min转速下搅拌混合均匀，升温至60℃，依次加入清净分散剂、抗氧剂、防锈剂、抗磨剂、摩擦改进剂、金属减活剂、抗泡剂，继续搅拌20min，最后加入粘度指数改进剂，继续搅拌40min，冷却至室温，即得。
对比例1
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯20份、壬二酸二(2-乙基己基)酯30份、季戊四醇油酸酯10份、聚α烯烃基础油40份、粘度指数改进剂6份、抗氧剂1份、清净分散剂3份、金属减活剂0.1份、防锈剂0.7份、抗磨剂2份、摩擦改进剂2份、抗泡剂0.03份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为实施例1所制备的噻二唑衍生物，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油；与实施例4的区别在于：改变了金属减活剂的重量份数。
对比例2
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯20份、壬二酸二(2-乙基己基)酯30份、季戊四醇油酸酯10份、聚α烯烃基础油40份、粘度指数改进剂6份、抗氧剂1份、清净分散剂3份、金属减活剂0.4份、防锈剂0.7份、抗磨剂2份、摩擦改进剂2份、抗泡剂0.03份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，金属减活剂为1,2,3-噻二唑-4-羧酸，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油；与实施例4的区别在于：将实施例1所得噻二唑衍生物替换为1,2,3-噻二唑-4-羧酸。
对比例3
一种长寿命汽车无极变速器油，包括以下重量份数的原料：二油酸新戊二醇酯20份、壬二酸二(2-乙基己基)酯30份、季戊四醇油酸酯10份、聚α烯烃基础油40份、粘度指数改进剂6份、抗氧剂1份、清净分散剂3份、防锈剂0.7份、抗磨剂2份、摩擦改进剂2份、抗泡剂0.03份，其中粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯共混物，聚异丁烯与聚甲基丙烯酸酯质量比为2:1，抗氧剂为4,4'-二辛基二苯胺，清净分散剂为硼化聚异丁烯基丁二酰亚胺，防锈剂为十二烯基丁二酸，抗磨剂为硫代磷酸三苯酯，摩擦改进剂为油酸乙二醇酯，抗泡剂为二甲基硅油；与实施例4的区别在于：不添加金属减活剂。
对比例1-3所述长寿命汽车无极变速器油均按照实施例4所述方法制备。
下面对实施例4-8、对比例1-3所制备的无极变速器油进行相关性能测试。抗磨减摩性能测试按照GB/T3142-1982(2004)《润滑剂承载能力测试法(四球法)》进行，使用MRS-10A微机控制四球摩擦试验机，其中测试温度为75℃，测试转速为1200r/min，测试时间为60min，测试负荷为392N，记录测试后的磨斑直径；牵引系数测试使用英国PCS MTM2 Mini-Traction Machine微牵引力测定仪进行测试，0.050以上为合格，其中油温加热条件为140℃，载荷为70N，平均滚动速度为3.8m/s，滑移率为5%；运动粘度测试按照ASTM D445-19规定进行；粘度指数测试按照ASTM D2270-04规定进行；氧化安定性测试按照SH/T0193-2008《润滑油氧化安定性的测定旋转氧弹法》进行，防腐蚀性测试按照NB/SH/T0517-2014《车辆齿轮油防锈性能的评定L-33-1法》进行；闪点按照ASTM D93-2020规定进行测定；倾点按照ASTMD97-2017规定进行测定；测试结果如表1所示。从表中可以看出，实施例4-8所制备的无极变速器油的抗磨减摩性能、牵引系数、运动粘度、粘度指数、氧化安定性、防锈性、闪点、倾点明显优于对比例1-3；从实施例4-6及对比例1的数据可以看出，无极变速器油中金属减活剂（实施例1所制备的噻二唑衍生物）的添加量能够显著影响油品的综合性能；从实施例4及对比例2的数据可以看出，对1,2,3-噻二唑-4-羧酸进行化学改性，得到噻二唑衍生物，并将其添加至无极变速器油，极大地提高了无极变速器油的抗磨减摩、防锈、抗氧化等性能。
表1无极变速器油性能测试结果
本发明通过两步法合成噻二唑衍生物，其具有极好的油溶性能，可以在润滑油中作为金属减活剂，还具有很好的极压抗磨特性。该噻二唑衍生物与混合煤制基础油及其它添加剂有良好的相容性、配伍性，各组分优化配比，协同增效，显著提高了油品的综合性能。本发明提供的汽车无极变速器油具有优异的抗磨减摩性、防锈性、抗氧化性、闪点和倾点，同时还具有较高的牵引系数和粘度指数，满足了现代汽车无极变速器润滑保护的要求，使用寿命能达到15-20万公里；此外，酯类全合成配方具有一定的生物降解性，能减少对环境的污染，适合大范围地推广和应用。
尽管已经示出和描述了本申请的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本申请的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本申请的范围由所附权利要求及其等同物限定。
Claims (10)
1.一种长寿命汽车无极变速器油，其特征在于，包括以下重量份数的原料：二油酸新戊二醇酯15-25份、壬二酸二(2-乙基己基)酯25-35份、季戊四醇油酸酯5-15份、聚α烯烃基础油35-45份、粘度指数改进剂4-10份、抗氧剂0.5-1.5份、清净分散剂1-5份、金属减活剂0.2-0.5份、防锈剂0.3-1.0份、抗磨剂1-3份、摩擦改进剂1-4份、抗泡剂0.01-0.05份，所述金属减活剂为噻二唑衍生物，噻二唑衍生物的制备方法如下：
S1、将3,3'-二硫代二丙酸分散于2-甲基四氢呋喃中，依次加入乙酸铬、1,2-环氧丁烷，升温至55-65℃，搅拌反应6-11h，过滤，取滤液，经减压蒸馏、干燥，得到中间体，中间体的结构式为：
；
S2、将步骤S1所得中间体分散于2-甲基四氢呋喃中，依次加入对甲苯磺酸、1,2,3-噻二唑-4-羧酸，升温至70-80℃，搅拌反应5-8h，过滤，取滤液，经减压蒸馏、萃取、浓缩、干燥，得到噻二唑衍生物，噻二唑衍生物的结构式为：
。
2.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，步骤S1中所述3,3'-二硫代二丙酸、乙酸铬、1,2-环氧丁烷的摩尔比为1:0.02-0.03:1.6-2.2，2-甲基四氢呋喃中3,3'-二硫代二丙酸的加入量为0.15-0.28g/mL。
3.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，步骤S2中所述中间体、对甲苯磺酸、1,2,3-噻二唑-4-羧酸的摩尔比为1:0.025-0.033:1.7-2.4，2-甲基四氢呋喃中中间体的加入量为0.20-0.25g/mL。
4.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，所述粘度指数改进剂为聚异丁烯、聚甲基丙烯酸酯、聚乙烯基正丁醚和苯乙烯-马来酸酐共聚物中的一种或两种以上。
5.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，所述抗氧剂为4,4'-二辛基二苯胺或2,4-二甲基-6-叔丁基苯酚。
6.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，所述清净分散剂为硼化聚异丁烯基丁二酰亚胺，防锈剂为十二烯基丁二酸。
7.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，所述抗磨剂为硫代磷酸三苯酯、亚磷酸二正丁酯、磷酸三甲酚酯中的一种或两种以上。
8.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，所述摩擦改进剂为油酸乙二醇酯、正十六烷胺和油酸酰胺中的一种或两种以上。
9.根据权利要求1所述的一种长寿命汽车无极变速器油，其特征在于，所述抗泡剂为二甲基硅油、乙基硅油、丙烯酸辛酯中的一种或两种以上。
10.根据权利要求1-9任一项所述的一种长寿命汽车无极变速器油的制备方法，其特征在于，包括以下步骤：将二油酸新戊二醇酯、壬二酸二(2-乙基己基)酯、季戊四醇油酸酯、聚α烯烃基础油混合均匀，升温至50-60℃，依次加入清净分散剂、抗氧剂、防锈剂、抗磨剂、摩擦改进剂、金属减活剂、抗泡剂，搅拌20-40min，最后加入粘度指数改进剂，继续搅拌40-60min，冷却至室温，即得。
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