CN107460022B - 一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法 - Google Patents

一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法 Download PDF

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CN107460022B
CN107460022B CN201710671609.5A CN201710671609A CN107460022B CN 107460022 B CN107460022 B CN 107460022B CN 201710671609 A CN201710671609 A CN 201710671609A CN 107460022 B CN107460022 B CN 107460022B
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严志军
严志宇
韩月
孙冰
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Abstract

本发明公开了一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法,将一定比例的硅的化合物和镁的化合物加入到反应釜中,用碱液调节pH,在密闭条件下进行水热合成反应;待反应结束后,将混合物抽滤、洗涤至中性并干燥,得到含纤蛇纹石粉体。称取上述制备的粉体置于烧瓶内,加水超声。在惰性气体保护下分别加入一定量的二价铁盐和三价铁盐,搅拌并水浴加热;逐滴加入碱液调节pH,反应结束后静置、抽滤、洗涤、干燥,得到纤蛇纹石/Fe3O4复合润滑油添加剂。本发明所述润滑油添加剂经修饰剂修饰后添加到基础油中能明显降低摩擦系数,提高抗磨性和稳定性,具有良好的减摩抗磨效果。

Description

一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的 方法
技术领域
本发明属于材料合成技术领域,具体涉及共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法。
背景技术
微纳米润滑油添加剂一直是摩擦领域研究中的重要方向,而矿物微粉作为其中的一类,当中最具有代表性的一种就是蛇纹石,它是一种分布很广的、典型的层状硅酸盐矿物之一,自然界中共有三种形态存在,分别为呈片状的利蛇纹石、槽状的叶蛇纹石和纳米管状的纤蛇纹石。天然蛇纹石矿物作为润滑油添加剂具有良好的减摩、抗磨、甚至自修复的特点,能够延长设备的使用寿命以及降低发动机功率损耗,成为近年来的研究热点。但天然蛇纹石在实际应用中由于其粒径很难达到要求,毒性、杂质伴生矿物多、纳米管直径不均匀等因素也限制了它的使用。
近年来,许多学者对天然蛇纹石的形成过程进行模拟,研究人工蛇纹石以克服天然蛇纹石的上述缺陷。对于纳米级别纤蛇纹石粒子的合成,一般比较常用的反应物为纳米二氧化硅、硅溶胶或硅酸镁等作为硅源,合成的水镁石、氧化镁方解石或氯化镁可溶盐等作为镁源。
由于Fe3O4具有磁性,可将其作为润滑油添加剂应用于润滑油中,且也是研究的热门,专利号CN103254971A的申请中公开了一种含有片状磁性纳米Fe3O4颗粒的润滑油及其制备方法,但其结果中摩擦系数较大。
发明内容
为解决上述现有技术中的问题,本发明提供一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法,提高润滑油的减摩抗磨性能,该方法工艺简单,可操作性强。
本发明共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法,包括以下步骤:
(1)称取一定比例的硅的化合物和镁的化合物,用碱液调节pH为10-14,密闭条件下进行水热合成反应;将反应产物抽滤、洗涤至中性并干燥,研磨得到含纤蛇纹石的粉体;
(2)称取上述步骤(1)制备的粉体加水超声分散;在惰性气体保护下分别加入一定量的二价铁盐和三价铁盐,搅拌并水浴加热;逐滴加入碱液调节pH为10-14,反应结束后静置将沉淀物抽滤、洗涤至中性,干燥,得到含纤蛇纹石和Fe3O4复合润滑油添加剂。
对于上文所述的技术方案,在优选的情况下,所述的水热合成的反应温度为180-300℃,反应时间为24-72h。
对于上文所述的技术方案,在优选的情况下,所述硅的化合物为滑石、硅溶胶、硅酸镁、气相白炭黑或沉淀水合二氧化硅。
对于上文所述的技术方案,在优选的情况下,所述镁的化合物为氧化镁、氯化镁、六水合氯化镁、氢氧化镁或碳酸镁。对于上文所述的技术方案,在优选的情况下,所述的硅的化合物和镁的化合物中Si/Mg摩尔比为0.07-7;
对于上文所述的技术方案,在优选的情况下,所述的惰性气体为N2
对于上文所述的技术方案,在优选的情况下,所述的碱液为NaOH溶液;NaOH溶液浓度为0.05-10mol/L。
对于上文所述的技术方案,在优选的情况下,所述的共沉淀反应中,水热合成反应制备的含纤蛇纹石粉体的添加量与铁盐的比例为0.1-1,超声时间为2-30min。
对于上文所述的技术方案,在优选的情况下,所述二价铁盐和三价铁盐是FeSO4·7H2O和 FeCl3
对于上文所述的技术方案,在优选的情况下,所述的二价铁盐和三价铁盐中Fe的摩尔比为0.05-5:1。
对于上文所述的技术方案,在优选的情况下,所述的共沉淀反应时间为0.5-3h,反应结束后静置0.5-3h。
对于上文所述的技术方案,在优选的情况下,所述的干燥条件为60-150℃、1-24h。
此外,本发明还涉及保护利用上文所述方法制备的含纤蛇纹石和Fe3O4复合润滑油添加剂。
与现有技术相比,本发明的有益效果体现在:
本发明共沉淀法制备的含纤蛇纹石和Fe3O4复合润滑油添加剂粉体,经司盘60和吐温60 修饰剂修饰后,添加到聚α烯烃合成基础油中进行四球摩擦磨损试验,来测试润滑油的抗摩擦性能及其抗磨损性能。经修饰剂修饰后,在基础油中具有良好的分散性和稳定性。在摩擦过程中,可使摩擦系数较基础油空白组大大地降低,摩擦系数和磨斑直径分别较基础油最多降低52%和58%。且复合粉体具有一定的磁性,随着摩擦过程的进行吸附在摩擦副表面的粉体,会在其表面形成一层抗摩擦膜从而实现降低磨损的目的。本发明合成的复合润滑油添加剂粉体较单一Fe3O4添加剂相比能更好地提升润滑油的减摩抗磨性能,具有良好的应用前景。
附图说明
图1是根据本发明实施例2中的一种复合粉体的XRD图。图示信息证明了复合润滑油添加剂粉体的成分为Fe3O4与含铁纤蛇纹石。
图2是根据本发明实施例1-3的摩擦系数曲线。图示中摩擦系数曲线很平稳,证明了复合润滑油添加剂粉体使摩擦过程很稳定且有效地降低了磨损。
图3是根据本发明实施例1-3的磨斑直径图。图示信息显示含纤蛇纹石和Fe3O4复合粉体用作润滑油添加剂时可使磨斑直径降低至400微米以下。
图4是根据本发明实施例2的磨斑表面微观形貌图。图示钢球表面微观形貌中的梨纹很浅,且磨斑较小,证明含纤蛇纹石和Fe3O4复合润滑油添加剂粉体具有很好的减摩抗磨效果。
具体实施方式
下述非限定性实施例可以使本领域的普通技术人员更全面地理解本发明,但不以任何方式限制本发明。
实施例1
1、将4.875g滑石和2.5gMgO加入到反应釜中,用2mol/L的NaOH调节溶液的pH至12,使混合液总体积为反应釜内聚四氟乙烯内衬体积的80%;将反应釜密封后放入250℃烘箱内反应30h;待反应结束后,将混合物抽滤、洗涤至中性,并放入100℃烘箱内干燥10h,得到含纤蛇纹石粉体。
2、称取上述制备的粉体5g置于烧瓶内,加水超声分散5min。在N2保护下分别加入3gFeSO4·7H2O和4.42gFeCl3,搅拌并在80℃水浴加热;逐滴加入NaOH溶液至pH为11,反应2h结束后静置1h,再将沉淀物抽滤、洗涤至中性,100℃干燥10h,得到含纤蛇纹石/Fe3O4复合润滑油添加剂。将上述制备的复合粉体、司盘60和吐温60修饰剂分别按1wt%、0.5wt%加入到50mL聚α烯烃合成基础油中,在75℃超声分散30min后进行四球摩擦磨损试验来测试润滑油的抗摩擦性能及其抗磨损性能。其中:摩擦副为四球摩擦副,载荷147N,主轴转速 1200rpm,温度75℃,摩擦时间60min。
实施例2
1、将1.17g滑石和0.6gMgO加入到反应釜中,用1mol/L的NaOH溶液调节pH至13,使混合液总体积为反应釜内聚四氟乙烯内衬体积的80%;将反应釜密封后放入220℃烘箱内反应30h;待反应结束后,将混合物抽滤、洗涤至中性110℃干燥8h,得到含纤蛇纹石粉体。
2、称取上述制备的粉体1.25g置于烧瓶内,加水超声分散15min。在N2保护下分别加入 2.87gFeSO4·7H2O和4.42gFeCl3,搅拌并在70℃水浴加热;逐滴加入NaOH溶液至pH为12,反应1h结束后静置0.5h,再将沉淀物抽滤、洗涤至中性,并放入110℃烘箱内干燥8h,得到含纤蛇纹石/Fe3O4复合润滑油添加剂。将上述制备的复合粉体、司盘60和吐温60修饰剂分别按1wt%、0.5wt%加入到50mL聚α烯烃合成基础油中,在75℃超声分散30min后进行四球摩擦磨损试验来测试润滑油的抗摩擦性能及其抗磨损性能。其中:摩擦副为四球摩擦副,载荷147N,主轴转速1200rpm,温度75℃,摩擦时间60min。
实施例3
1、将2.925g滑石和1.5gMgO加入到反应釜中,用3mol/L的NaOH溶液调节pH至13.5,使混合液总体积为反应釜内聚四氟乙烯内衬体积的80%;将反应釜密封后放入220℃烘箱内反应60h;待反应结束后,将混合物抽滤、洗涤至中性105℃干燥9h,得到含纤蛇纹石粉体。
2、称取上述制备的粉体2.5g置于烧瓶内,加水超声分散20min。在N2保护下分别加入 3.15gFeSO4·7H2O和4.42gFeCl3,搅拌并在90℃水浴加热;逐滴加入NaOH溶液至pH为13,反应3h结束后静置1.5h,再将沉淀物抽滤、洗涤至中性,并放入105℃烘箱内干燥9h,得到含纤蛇纹石/Fe3O4复合润滑油添加剂。将上述制备的复合粉体、司盘60和吐温60修饰剂分别按1wt%、0.5wt%加入到50mL聚α烯烃合成基础油中,在75℃超声分散30min后进行四球摩擦磨损试验来测试润滑油的抗摩擦性能及其抗磨损性能。其中:摩擦副为四球摩擦副,载荷147N,主轴转速1200rpm,温度75℃,摩擦时间60min。

Claims (7)

1.一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法,其特征在于:包括以下步骤:
(1)称取一定比例的硅的化合物和镁的化合物,用碱液调节pH为10-14,密闭条件下进行水热合成反应;将反应产物抽滤、洗涤至中性并干燥,研磨得到含纤蛇纹石的粉体;
(2)称取上述步骤(1)制备的粉体加水超声分散;在惰性气体保护下分别加入一定量的二价铁盐和三价铁盐,搅拌并水浴加热;逐滴加入碱液调节pH为10-14,反应结束后静置将沉淀物抽滤、洗涤至中性,干燥,得到含纤蛇纹石和Fe3O4复合润滑油添加剂;
其中,所述硅的化合物为滑石、硅溶胶、硅酸镁、气相白炭黑或沉淀水合二氧化硅;所述镁的化合物为氧化镁、氯化镁、六水合氯化镁、氢氧化镁或碳酸镁;所述二价铁盐和三价铁盐是FeSO4·7H2O和FeCl3
2.根据权利要求1所述的制备方法,其特征在于:所述的硅的化合物和镁的化合物中Si/Mg摩尔比为0.07-7。
3.根据权利要求1所述的制备方法,其特征在于:所述的水热合成的反应温度为
180-300℃,反应时间为24-72h。
4.根据权利要求1所述的制备方法,其特征在于:所述的二价铁盐和三价铁盐中Fe 的摩尔比为0.05-5。
5.根据权利要求1所述的制备方法,其特征在于:所述的共沉淀反应中,水热合成反应制备的含纤蛇纹石粉体的添加量与铁盐的比例为0.1-1。
6.根据权利要求1所述的制备方法,其特征在于:所述的共沉淀反应时间为0.5-3h,反应结束后静置0.5-3h;所述的干燥条件为60-150℃、1-24h。
7.利用权利要求1所述方法制备的含纤蛇纹石和Fe3O4复合润滑油添加剂。
CN201710671609.5A 2017-08-08 2017-08-08 一种共沉淀法制备含纤蛇纹石和Fe3O4复合润滑油添加剂的方法 Expired - Fee Related CN107460022B (zh)

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