CN108690678A - 一种含石墨烯的润滑油的制备方法 - Google Patents
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Abstract
本发明公开了一种含石墨烯的润滑油的制备方法,包括如下步骤:A.将原料石墨烯离心分离,取上层液,低温干燥得到离心分离后的石墨烯粉末;B.将上述离心分离后的石墨烯粉末真空下烘干形成粗成品;C.将上述粗成品与添加剂混合形成混合物W,溶于加热溶剂中搅拌均匀,然后趁热过滤,滤液真空加热干燥,得到成品Q;D.将上述成品Q作为成分之一,配置石墨烯润滑液,重量百分比成分如下:成品Q1%‑3%,助剂1‑5%,基础油为余量。配方中的石墨烯由于经过预处理,在配方中表现出较好的稳定性。
Description
技术领域
本发明属于润滑技术领域,特别涉及一种含石墨烯的润滑油的制备方法。
背景技术
石墨烯是由碳原子通过SP2杂化组成的呈六角蜂巢状二维网格结构的一种新型炭材料,其厚度仅为0.335nm,是目前世界上最薄的纳米材料。单层石墨烯拥有2600m2/g的大比表面积,被认为是目前材料领域中最坚硬的材料,其断裂强度可达41N.m-1,自身的机械延展25%,杨氏模量1TPa。由于石墨烯优良的机械性能和微小的片层间的剪切力,导致其具有比石墨更低的摩擦系数,优异的减磨润滑性能。
但是石墨烯作为润滑油中关键成分,由于其极性溶剂中溶解度极低,容易出现与其他成分不兼容、分散不均的问题,从而严重影响润滑油的性能。现有技术中有针对石墨烯进行亲油性的改性,但是改性后的石墨烯在一些商用成品润滑油中的分散仍然难以实现稳定分散的效果。
发明内容
本发明的目的在于克服现有技术的补足,提供一种含石墨烯的润滑油的制备方法,解决现有润滑油无法实现石墨烯均匀分散和稳定性差的技术问题。
为了实现上述发明目的,本发明的技术方案如下:
一种含石墨烯的润滑油的制备方法,包括如下步骤:
A.将原料石墨烯离心分离,取上层液,低温干燥得到离心分离后的石墨烯粉末;
B.将上述离心分离后的石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与添加剂混合形成混合物W,溶于加热溶剂中搅拌均匀,然后趁热过滤,滤液真空加热干燥,得到成品Q;
D.将上述成品Q作为成分之一,配置石墨烯润滑液,重量百分比成分如下:
成品Q 1%-3%;
助剂 1-5%;
基础油 余量;
其中
粗成品与添加剂的质量比为1:0.1~100:0.1;
添加剂为二碘辛烷或氯萘;
成品Q占混合物W的50-85wt%。
进一步的,所述含石墨烯的润滑油的制备方法,其中所述离心分离的离心力是4000-8000×g。
进一步的,所述含石墨烯的润滑油的制备方法,其中所述溶剂为氯苯、二氯苯、三氯苯、二甲苯或三甲苯的一种。
进一步的,所述含石墨烯的润滑油的制备方法,其中所述离心分离后的石墨烯粉末层数可选对象为1~6层。
进一步的,所述含石墨烯的润滑油的制备方法,其中所述过滤,使用的孔径为0.45-1微米。
进一步的,所述含石墨烯的润滑油的制备方法,其中所述助剂为烷基苯磺酸钠、C8-C22的脂肪酸盐、烷基硫酸盐或脂肪醇聚氧乙烯基醚的一种。
进一步的,所述的含石墨烯的润滑油的制备方法,其中所述基础油为矿物油、植物油或合成油的一种。
与现有技术相比,本发明具有以下有益效果:
在制备石墨烯润滑油组合物前,对石墨烯进行预处理,可以提升润滑油的稳定性和分散性;并且配方的稳定性和分散性能与石墨烯的层数、是否过滤关系密切。
具体实施方式
以下结合具体实施例来进一步说明本发明,但实施例并不对本发明做任何形式的限定。除非特别说明,本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明,以下实施例所用试剂和材料均为市购。
实施例1
一种含石墨烯的润滑油的制备方法,包括如下步骤:
A.将原料石墨烯在4000×g下离心分离,取上层液,低温干燥得到2-4层的石墨烯粉末;
B.将上述石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与二碘辛烷混合形成混合物W,粗成品与二碘辛烷的质量比为1:0.1;溶于120℃氯苯中搅拌均匀,然后趁热用0.45微米滤头过滤,滤液真空加热干燥,得到成品Q。经计算成品Q占混合物W的50%。
D.将上述成品Q作为成分之一,配置石墨烯润滑液,重量百分比成分如下:
成品Q 1%
烷基苯磺酸盐 1%
矿物油 余量
实施例2
一种含石墨烯的润滑油的制备方法,包括如下步骤:
A.将原料石墨烯在6000×g下离心分离,取上层液,低温干燥得到1-5层的石墨烯粉末;
B.将上述石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与氯萘混合形成混合物W,粗成品与氯萘的质量比为10: 0.1;溶于120℃三甲苯中搅拌均匀,然后趁热用0.45微米滤头过滤,滤液真空加热干燥,得到成品Q。经计算成品Q占混合物W的62%。
D.将上述成品Q作为成分之一,配置石墨烯润滑油,重量百分比成分如下:
成品Q 2%
脂肪醇聚氧乙烯基醚 2%
植物油 余量
实施例3
一种含石墨烯的润滑油的制备方法,包括如下步骤:
A.将原料石墨烯在8000×g下离心分离,取上层液,低温干燥得到3-6层的石墨烯粉末;
B.将上述石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与二碘辛烷混合形成混合物W,粗成品与二碘辛烷的质量比为50:0.1;溶于120℃二氯苯中搅拌均匀,然后趁热用0.75微米滤头过滤,滤液真空加热干燥,得到成品Q。经计算成品Q占混合物W的75%。
D.将上述成品Q作为成分之一,配置石墨烯润滑油,重量百分比成分如下:
成品Q 3%
烷基硫酸盐 5%
合成油 余量
实施例4
一种含石墨烯的润滑油的制备方法,包括如下步骤:
A.将原料石墨烯在8000×g下离心分离,取上层液,低温干燥得到3-6层的石墨烯粉末;
B.将上述石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与氯萘混合形成混合物W,粗成品与氯萘的质量比为100: 0.1;溶于140℃三甲苯中搅拌均匀,然后趁热用1微米滤头过滤,滤液真空加热干燥,得到成品Q。经计算成品Q占混合物W的85%。
D.将上述成品Q作为成分之一,配置石墨烯润滑油,重量百分比成分如下:
成品Q 2%
烷基硫酸盐 5%
植物油 余量
实施例5
一种含石墨烯的润滑油的制备方法,包括如下步骤:
A.将原料石墨烯在6000×g下离心分离,取上层液,低温干燥得到3-5层的石墨烯粉末;
B.将上述石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与氯萘混合形成混合物W,粗成品与氯萘的质量比为100: 0.1;溶于130℃三甲苯中搅拌均匀,然后趁热用1微米滤头过滤,滤液真空加热干燥,得到成品Q。经计算成品Q占混合物W的80%。
D.将上述成品Q作为成分之一,配置石墨烯润滑油,重量百分比成分如下:
成品Q 3%
C8的脂肪酸盐 4%
植物油 余量
实施例6
实施例1中所给出了石墨烯制备步骤及润滑油配方。润滑油性能表现和稳定性如下表所示。作为对比,我们设立了对比实验A-C。对比实验A中,用等量的未经离心的石墨烯代替成品Q,其余组分不变;对比实验B中,用等量的混合物W代替成品Q,其余组分不变。对比实验C中,离心力选为2000×g,离心后的石墨烯层数为10-20层,其余步骤不变。
实施例7
实施例2中所给出了石墨烯制备步骤及润滑油配方。润滑油性能表现和稳定性如下表所示。作为对比,我们设立了对比实验D-F。对比实验D中,用等量的未经离心的石墨烯代替成品Q,其余组分不变;对比实验E中,用等量的混合物W代替成品Q,其余组分不变。对比实验F中,离心力选为1000×g,离心后的石墨烯层数为15-30层,其余步骤不变。
实施例8
实施例5中所给出了石墨烯制备步骤及润滑油配方。润滑油性能表现和稳定性如下表所示。作为对比,我们设立了对比实验G-I。对比实验G中,用等量的未经离心的石墨烯代替成品Q,其余组分不变;对比实验H中,用等量的混合物W代替成品Q,其余组分不变。对比实验I中,离心力选为500×g,离心后的石墨烯层数为5-100层,其余步骤不变。
由以上对比实验数据可知,配方的稳定性和分散性能与石墨烯的层数、是否过滤关系密切。按说明书所述步骤预处理后的石墨烯作为润滑油配方,稳定性能显著提升。
Claims (5)
1.一种含石墨烯的润滑油的制备方法,其特征在于,包括如下步骤:
A.将原料石墨烯离心分离,取上层液,低温干燥得到离心分离后的石墨烯粉末;
B.将上述离心分离后的石墨烯粉末真空下烘干形成粗成品;
C.将上述粗成品与添加剂混合形成混合物W,溶于加热溶剂中搅拌均匀,然后趁热过滤,滤液真空加热干燥,得到成品Q;
D.将上述成品Q作为成分之一,配置石墨烯润滑液,重量百分比成分如下:
成品Q 1%-3%;
助剂 1-5%;
基础油 余量;
其中,粗成品与添加剂的质量比为1:0.1~100:0.1;
添加剂为二碘辛烷或氯萘;
成品Q占混合物W的 50-85wt%。
2.如权利要求1所述一种含石墨烯的润滑油的制备方法,其特征在于,所述离心分离的离心力是4000- 8000×g。
3.如权利要求1所述一种含石墨烯的润滑油的制备方法,其特征在于,所述溶剂为氯苯、二氯苯、三氯苯、二甲苯或三甲苯的一种。
4.如权利要求1所述一种含石墨烯的润滑油的制备方法,其特征在于,离心分离后的石墨烯粉末层数为1~6层。
5.如权利要求1所述一种含石墨烯的润滑油的制备方法,其特征在于,所述过滤,使用的孔径为0.45-1微米。
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