CN101270313B - 片状纳米石墨润滑油添加剂的制备方法 - Google Patents

片状纳米石墨润滑油添加剂的制备方法 Download PDF

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CN101270313B
CN101270313B CN2008100548218A CN200810054821A CN101270313B CN 101270313 B CN101270313 B CN 101270313B CN 2008100548218 A CN2008100548218 A CN 2008100548218A CN 200810054821 A CN200810054821 A CN 200810054821A CN 101270313 B CN101270313 B CN 101270313B
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张瑞军
杨育林
齐效文
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Yanshan University
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Abstract

本发明公开一种片状纳米石墨润滑油添加剂的制备方法。所述片状纳米石墨润滑油添加剂是以高纯天然石墨为原料,采用重复插层膨化处理技术,制备膨化程度均匀的膨胀石墨;采用超声波振荡技术对膨胀石墨进行振荡破碎,制备片状纳米石墨粉体;将一定量片状纳米石墨粉体添加至润滑油中,以改善机械零部件的摩擦磨损行为。

Description

片状纳米石墨润滑油添加剂的制备方法
技术领域
本发明涉及一种片状纳米石墨润滑油添加剂的制备方法。该添加剂材料添加在润滑油中,能够表现出优异的减摩抗磨性能,从而有效延缓摩擦副的使用寿命。
背景技术
能源与环境是经济社会持续发展的两大主题。对于机械零部件而言,摩擦磨损是在所难免的。机械部件的摩擦磨损在带来材料和能源大量损耗的同时,还会造成十分严重的环境污染。在润滑油中加入摩擦学添加剂是有效减缓机械零部件摩擦磨损、降低能量损耗的重要技术手段之一。
以石墨、金刚石为代表的碳材料在摩擦学添加剂领域已得到广泛应用。近来的许多研究工作表明,利用纳米材料的比表面积大、高扩散性和熔点低等突出特点,将碳材料纳米化,能够进一步提高碳材料作为摩擦学添加剂的减摩抗磨性能。例如,王艳辉等在“纳米金刚石在摩擦副界面的减摩耐磨机理探讨”的文章中指出(金刚石与磨料磨具工程,2001,4(124):4~10.),在钢铁材料摩擦副之间加入含纳米金刚石颗粒的润滑油,可使摩擦系数降低约50%,动力消耗明显减少;中国专利(公开号:CN 1632082A.)公开的一种含有纳米片状石墨的润滑油,将片状纳米石墨添加至润滑油中,有效地提高了润滑油的减摩抗磨能力和承载能力。
最近,陈国华(Guohua Chen,Wengui Weng,Dajun Wu,et al.Preparation and characterization of graphite nanosheets fromultrasonic powdering technique.Carbon,2004,42:753~759.)等提出以膨胀石墨为原料,用超声波粉碎制备纳米石墨薄片的方法。其原理是利用液相中形成的空化气泡,冲击并加速固体颗粒的摩擦,进而产生脆性颗粒的粉碎,进而形成厚度为纳米尺度的石墨薄片。但是由于天然石墨插层处理不充分,导致膨胀石墨膨化程度不均匀,所获纳米石墨薄片厚度差异很大。
发明内容
为了克服现有技术存在的上述不足,本发明提供一种片状纳米石墨润滑油添加剂的制备方法,该发明以高纯天然石墨为原料,采用重复插层膨化处理技术,制备膨化程度均匀的膨胀石墨;采用超声波振荡技术对膨胀石墨进行振荡破碎,制备片状纳米石墨粉体;将一定量片状纳米石墨粉体添加至润滑油中,以改善机械零部件的摩擦磨损行为。
这种纳米膨胀石墨润滑添加剂的制备方法是:
(1)一次膨胀石墨的制备:对35-80目的天然鳞片石墨进行插层处理,插层剂为浓度90~98%的浓硫酸,氧化剂是浓度25~40%的过氧化氢,在20~30℃的温度下插层处理10~20分钟,随后,将插层后的产物水洗至PH值7~8,之后,再在80~100℃下烘干1.5~2.5小时,在800~1000℃的温度下进行高温膨化处理,获得一次膨胀石墨。
(2)膨胀石墨蠕虫的制备:再以一次膨胀石墨为原料,采用与前述相同的插层处理工艺再次进行插层、水洗、高温膨化处理,制得膨胀石墨蠕虫;
(3)片状纳米石墨粉体的制备:采用膨胀石墨蠕虫为原材料,在超声波振荡仪中进行振荡破碎处理。超声振荡破碎时,采用乙醇为分散溶剂,膨胀石墨蠕虫与乙醇溶剂的质量比为1∶50~1∶300,振荡时间为3~10小时;振荡破碎结束后,即可获得用作润滑油添加剂的片状纳米石墨粉体。
本发明的有益效果是:片状纳米石墨作为润滑添加剂,能够显著改善机械零部件的摩擦磨损行为,减少材料损失和能源消耗。
具体实施方式
(a)一次膨胀石墨的制备:在实验室条件下,采用化学法制备膨胀石墨。其中,所用原料是粒度为50目的天然鳞片石墨(纯度:99.9%,产地:山东南墅石墨公司),插层剂为浓度98%的浓硫酸,氧化剂是浓度30%的过氧化氢。在约25℃的室温下插层处理10分钟,随后,将插层后的产物水洗至PH值8,之后,再在100℃下烘干2小时,在800℃的温度下进行高温膨化处理,获得膨胀倍数约200倍的一次膨胀石墨。
(b)膨胀石墨蠕虫的制备:再以一次膨胀石墨为原料,同样采用浓度98%的浓硫酸为插层剂,浓度30%的过氧化氢为氧化剂,在约25℃的室温下插层处理8分钟,之后再将插层后的产物水洗至PH值8,并在100℃下烘干2小时,最后在800℃的温度下再次进行高温膨化处理,制得本发明用膨胀石墨蠕虫。
(c)片状纳米石墨粉体(润滑油添加剂)的制备:在实验室条件下,采用膨胀石墨蠕虫为原材料,在KQ118型超声波振荡仪(昆山市超声仪器有限公司)中进行振荡破碎处理。超声振荡破碎时,采用乙醇为分散溶剂,膨胀石墨蠕虫与乙醇溶剂的质量比为1∶150,振荡时间为6小时。振荡破碎结束后,获得粒径不大于20μm,厚度为10~20nm的片状纳米石墨粉体,即本发明的片状纳米石墨润滑油添加剂。
(d)润滑剂配制:在SJ 15W-40型昆仑润滑油中添加2%(以质量分数计)的片状纳米石墨润滑油添加剂,调配成润滑剂。为确保片状纳米石墨粉体在润滑油中充分分散,采用山梨糖醇酐油酸酯为分散剂。
(e)摩擦学性能评价:
采用MMU-5G型万能摩擦磨损试验机进行摩擦学试验。其中,实验载荷为200牛顿,转速为300转/分,试验时间为1小时,两种对磨材料分别为喷钼合金涂层和45#钢。不同温度摩擦学试验结果如表1所示。
表1不同温度下片状纳米石墨润滑油添加剂的摩擦学试验结果
Figure GSB00000400671600031
实验结果表明:与纯基础油相比,润滑油中添加本发明的片状纳米石墨润滑添加剂时,在较高载荷下,常温和高温均具有明显的减摩抗磨效应。

Claims (1)

1.一种片状纳米石墨润滑油添加剂的制备方法,其特征是:所述方法包括如下步骤:
(1)一次膨胀石墨的制备:对35~80目的天然鳞片石墨进行插层处理,插层剂为浓度90~98%的浓硫酸,氧化剂是浓度25~40%的过氧化氢,在20~30℃的温度下插层处理10~20分钟,随后,将插层后的产物水洗至PH值7~8,之后,再在80~100℃下烘干1.5~2.5小时,在800~1000℃的温度下进行高温膨化处理,获得一次膨胀石墨;
(2)膨胀石墨蠕虫的制备:再以一次膨胀石墨为原料,采用与前述相同的插层处理工艺再次进行插层、水洗、高温膨化处理,制得膨胀石墨蠕虫;
(3)片状纳米石墨粉体的制备:采用膨胀石墨蠕虫为原材料,在超声波振荡仪中进行振荡破碎处理;超声振荡破碎时,采用乙醇为分散溶剂,膨胀石墨蠕虫与乙醇溶剂的质量比为1∶50~1∶300,振荡时间为3~10小时;振荡破碎结束后,即可获得用作润滑油添加剂的片状纳米石墨粉体。
CN2008100548218A 2008-04-18 2008-04-18 片状纳米石墨润滑油添加剂的制备方法 Expired - Fee Related CN101270313B (zh)

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CN101003369A (zh) * 2007-01-17 2007-07-25 大连理工大学 爆轰制备片状纳米石墨粉的方法

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