CN108441283B - 一种石墨烯润滑油及其制备方法 - Google Patents
一种石墨烯润滑油及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种石墨烯润滑油及其制备方法，所述石墨烯润滑油按重量份包括如下组分：基础油80‑90份；含石墨烯的鸡蛋油10‑15份；助剂2‑14份。所述含石墨烯的鸡蛋油制备方法，包括以下步骤：1)将鸡蛋煮熟，取蛋黄捣碎后，向其中加入氧化石墨烯，混合均匀，得石墨烯蛋黄拌合料；2)、将石墨烯蛋黄拌合料置于铁锅中，翻炒至蛋黄熬出油后，选择性加入油酸，继续翻炒10min，然后自然冷却至30～50摄氏度，于30～50摄氏度下低速离心，去沉淀，留液体，即为含石墨烯的鸡蛋油。本发明能够有效改善石墨烯的分散稳定性，提高汽车发动机的润滑性。
Description
技术领域
本发明涉及润滑油领域，具体涉及一种石墨烯润滑油及其制备方法。
背景技术
发动机的润滑性能与汽车的安全、环保以及节能等性能息息相关，随着发动机性能的不断提高，对润滑方面的要求日趋复杂、苛刻，而氧化石墨烯作为一种具有二维结构的碳质新材料，具有较高的比表面积、导热性和力学性能等一系列优异的性质，因此，为了改善发动机润滑性能、实现减磨节能，需要往润滑油中添加一定量的石墨烯，但是，如何防止添加有氧化石墨烯的润滑油产生分层、沉淀、以及提高其储存温度性，是研究者必须要面对的技术问题。
发明内容
本发明的目的在于克服现有技术的缺陷，提供一种石墨烯润滑油及其制备方法，以改善石墨烯的分散稳定性，提高汽车发动机的润滑性。
为了实现上述目的，本发明采取的技术方案如下：
技术方案一：
一种石墨烯润滑油，按重量份包括如下组分：
基础油 80-90份；
含石墨烯的鸡蛋油 10-15份；
助剂 2-14份。
进一步的，所述含石墨烯的鸡蛋油制备方法，包括以下步骤：
步骤1、将鸡蛋煮熟，取蛋黄捣碎后，向其中加入氧化石墨烯，混合均匀，得石墨烯蛋黄拌合料；
步骤2、将步骤1制得的石墨烯蛋黄拌合料置于铁锅中，翻炒至蛋黄熬出油后，选择性加入油酸，继续翻炒10min，然后自然冷却至30～50摄氏度，于30～50摄氏度下低速离心，去沉淀，留液体，所述液体即为含石墨烯的鸡蛋油。
更进一步的，步骤2所述低速离心的转速为3000～5000转/分钟。
更进一步的，步骤1中氧化石墨烯的加入量为：蛋黄与氧化石墨烯质量比5～12：1。
更进一步的，步骤2中油酸的加入量为蛋黄与油酸质量比5～12：2。
更进一步的，步骤1中所述氧化石墨烯采用少层氧化石墨烯。
进一步的，所述助剂包括分散剂，黏度调节剂，抗泡剂，抗氧化剂，防锈剂中的一种或几种。
更进一步的，所述分散剂为硬脂酸、十二烷基苯磺酸钠、脂肪酸甘油酯、三聚甘油单月桂酸酯、硬脂酸单甘油酯、季铵化物中的一种或几种；
所述黏度调节剂为聚甲基丙烯酸酯、烯烃共聚物、氢化苯乙烯-双烯共聚物、乙丙共聚物中的一种或几种；
所述抗泡剂为烯甘油醚、二甲基硅油、乳化硅油和高碳醇脂肪酸酯复合物中的一种或几种；
所述抗氧化剂为双十二碳醇酯、三辛酯中的一种或两种；
所述防锈剂为石油磺酸钡、石油磺酸钠、二壬基萘磺酸钡、羊毛脂、蜂蜡、油酸十八烷胺和苯并三氮唑中的一种或几种。
进一步的，所述基础油为矿物油、液体石蜡、聚α-烯烃、酯类油和聚醚类油中的一种或几种。
更进一步的，所述少层氧化石墨烯的层数小于等于3层。
更进一步的，所述少层氧化石墨烯的制备方法包括以下步骤：采用Hummer法，在一个250mL的烧杯中加入2g鳞片石墨粉末，冰水浴的条件下向其中加入1gNaNO3后加入46mL质量浓度为98％的H2SO4并充分搅拌后，缓慢加入6gKMnO4，保持溶液的温度在20摄氏度至少5min，然后加热到35摄氏度，保持30min；加入92mL的水，再搅拌15min，温度将会升高到约98摄氏度；然后加入80mL的60摄氏度体积浓度为3％的双氧水，7200转/分钟的转速下离心30min，用60摄氏度的热水清洗残渣直至上层悬浮液的pH为7，把得到的粉末再次分散到水中，超声15min，过滤掉黑色残留物后得到均一的悬浮液，然后喷雾干燥后得少层氧化石墨烯。
技术方案二：
一种石墨烯润滑油的制备方法，包括以下步骤：
按重量份称取各原料后，将含石墨烯的鸡蛋油和助剂加入到基础油中，采用高速搅拌机于100～120摄氏度、1200～1500转/分钟的转速下均质搅拌3～6小时至混合均匀，即得。
与现有技术相比，本发明所取得的有益效果如下：
1、采用本发明方法制备的少层氧化石墨烯更易于通过鸡蛋油进行改性，从而提高石墨烯润滑油的分散性、储藏稳定性以及减磨抗磨性能，从而节约能耗。
2、本发明中先将氧化石墨烯与蛋黄拌合后再熬制鸡蛋油，能够实现石墨烯的改性，从而提高石墨烯润滑油的分散性、储藏稳定性以及减磨抗磨性能，从而节约能耗。
3、本发明含石墨烯的鸡蛋油在制备过程中采用3000～5000转的速度进行低速离心，有利于将熬制鸡蛋油过程中产生的残渣进行沉淀，而将氧化石墨烯则留存于鸡蛋油中。
4、本发明在鸡蛋油的熬制过程中加入油酸，能够提高石墨烯在鸡蛋油中的浓度及分散稳定性，减少离心过程中石墨烯的损失，节约了成本。
本发明方法制备润滑油过程中各个参数均起到关键性的作用，采用本发明方法制得的润滑油能够有效改善石墨烯的分散稳定性，提高汽车发动机的润滑性，从而节约因摩擦而产生的能耗。
具体实施方式
以下结合实施例对本发明进行进一步详细的叙述。
本发明中聚α-烯烃PAO8购自上海道普化学国际贸易有限公司。
本发明中所用少层氧化石墨烯的制备方法为：采用Hummer法，在一个250mL的烧杯中加入2g鳞片石墨粉末，冰水浴的条件下向其中加入1gNaNO3后加入46mL质量浓度为98％的H2SO4并充分搅拌后，缓慢加入6gKMnO4，保持溶液的温度在20摄氏度至少5min，然后加热到35摄氏度，保持30min；加入92mL的水，再搅拌15min，温度将会升高到约98摄氏度；然后加入80mL的60摄氏度体积浓度为3％的双氧水，7200转/分钟的转速下离心30min，用60摄氏度的热水清洗残渣直至上层悬浮液的pH为7，把得到的粉末再次分散到水中，超声15min，过滤掉黑色残留物后得到均一的悬浮液，然后喷雾干燥后得少层石墨烯。
实施例1
一种石墨烯润滑油，按重量份包括如下组分：
其制作方法为：
步骤一、将鸡蛋煮熟，取蛋黄捣碎后，按蛋黄与少层氧化石墨烯质量比8：1，向其中加入氧化石墨烯，混合均匀，得石墨烯蛋黄拌合料；
步骤二、将步骤一制得的石墨烯蛋黄拌合料置于铁锅中，翻炒至蛋黄熬出油后，继续翻炒10min，然后自然冷却至40摄氏度，于40摄氏度下低速离心，去沉淀，留液体，所述液体即为含石墨烯的鸡蛋油，所述低速离心的转速为4000转/分钟；
步骤三、按重量份称取各原料，将含石墨烯的鸡蛋油、分散剂、黏度调节剂、抗泡剂、抗氧化剂加入到基础油中，采用高速搅拌机于110摄氏度、1300转/分钟的转速下均质搅拌5小时至混合均匀，即得。
实施例2
一种石墨烯润滑油，按重量份包括如下组分：
其制作方法为：
步骤一、将鸡蛋煮熟，取蛋黄捣碎后，按蛋黄与少层氧化石墨烯质量比10：1，向其中加入氧化石墨烯，混合均匀，得石墨烯蛋黄拌合料；
步骤二、将步骤一制得的石墨烯蛋黄拌合料置于铁锅中，翻炒至蛋黄熬出油后，按蛋黄与油酸质量比10：2，向其中加入油酸，继续翻炒10min，然后自然冷却至40摄氏度，于40摄氏度下低速离心，去沉淀，留液体，所述液体即为含石墨烯的鸡蛋油，所述低速离心的转速为4000转/分钟；
步骤三、按重量份称取各原料，将含石墨烯的鸡蛋油、分散剂、黏度调节剂、抗泡剂、抗氧化剂加入到基础油中，采用高速搅拌机于110摄氏度、1300转/分钟的转速下均质搅拌5小时至混合均匀，即得。
对比例1
一种石墨烯润滑油，按重量份包括如下组分：
其制作方法为：
步骤一、将鸡蛋煮熟，取蛋黄捣碎后，置于铁锅中，翻炒至蛋黄熬出油后，继续翻炒10min，然后自然冷却至40摄氏度，于40摄氏度下低速离心，去沉淀，留液体，所述液体即为鸡蛋油，所述低速离心的转速为4000转/分钟；
步骤二、向步骤一制得的鸡蛋油中加入少层氧化石墨烯和油酸，于铁锅中于搅拌条件下炒制10min后，即得含石墨烯的鸡蛋油；
步骤三、按重量份称取各原料，将步骤二制得的含石墨烯的鸡蛋油、油酸、分散剂、黏度调节剂、抗泡剂、抗氧化剂加入到基础油中，采用高速搅拌机于110摄氏度、1300转/分钟的转速下均质搅拌5小时至混合均匀，即得。
对比例2
一种石墨烯润滑油，按重量份包括如下组分：
其制作方法为：
按重量份称取各原料，将少层氧化石墨烯、分散剂、黏度调节剂、抗泡剂、抗氧化剂加入到基础油中，采用高速搅拌机于110摄氏度、1300转/分钟的转速下均质搅拌5小时至混合均匀，即得。
效果例1
储存稳定性测试：
方法：将实施例和对比例制得的目标产物润滑油分别静置0天、15天、30天、60天和180、360天后，观察目标产物润滑油的团聚、分层、沉淀现象，结果见表1；
外观评价标准：
1、分散稳定，无团聚、分层、沉淀现象；
2、分散较稳定，有轻微的团聚、分层、沉淀现象；
3、分散不稳定，有明显团聚、分层、沉淀现象；
4、分散极不稳定，有严重的团聚、分层、沉淀现象；
表1 各实施例和对比例制得的润滑油储存后团聚、分层、沉淀情况
| 0天 | 15天 | 30天 | 60天 | 180天 | 360天 | |
| 实施例1 | 1 | 1 | 1 | 1 | 1 | 2 |
| 实施例2 | 1 | 1 | 1 | 1 | 1 | 1 |
| 对比例1 | 1 | 1 | 2 | 3 | 3 | 4 |
| 对比例2 | 1 | 1 | 2 | 3 | 4 | 4 |
从表中数据可以看出，实施例1和2中在基础油中加入采用本发明方法制备的含石墨烯的鸡蛋油后制得的润滑油，其团聚、分层、沉淀情况明显优于对比例1和对比例2中的方法制备的润滑油，采用本发明方法制备的润滑油储存稳定性明显提高。
效果例2
减磨抗磨性能测试：按照SH/T 0189-92进行，采用夏门天机MS-10J四球摩擦损试验机，电机转速1200±50r/min，温度室温，负荷392N，时间60min，磨斑直径和摩擦系数结果见表2。
表2 各实施例和对比例制得的润滑油的磨斑直径和摩擦系数
| WSD(mm) | μ | |
| 实施例1 | 0.508 | 0.077 |
| 实施例2 | 0.502 | 0.074 |
| 对比例1 | 0.677 | 0.082 |
| 对比例2 | 0.682 | 0.089 |
从表中数据可以看出，实施例1和2中在基础油中加入采用本发明方法制备的含石墨烯的鸡蛋油后制得的润滑油，其磨斑直径和摩擦稀释明显小于对比例1和对比例2中的方法制备的润滑油，采用本发明方法制备的润滑油减磨抗磨性能明显提高，因此采用本发明方法制备的润滑油能有效减少因摩擦而产生的能力损耗。
以上所述实施方式仅为本发明的优选实施例，而并非本发明可行实施的穷举。对于本领域一般技术人员而言，在不背离本发明原理和精神的前提下对其所作出的任何显而易见的改动，都应当被认为包含在本发明的权利要求保护范围之内。
Claims (9)
1.一种石墨烯润滑油，其特征在于，按重量份包括如下组分：
基础油 80-90份；
含石墨烯的鸡蛋油 10-15份；
助剂 2-14份；
所述含石墨烯的鸡蛋油制备方法，包括以下步骤：
步骤1、将鸡蛋煮熟，取蛋黄捣碎后，向其中加入氧化石墨烯，混合均匀，得石墨烯蛋黄拌合料；
步骤2、将步骤1制得的石墨烯蛋黄拌合料置于铁锅中，翻炒至蛋黄熬出油后，选择性加入油酸，继续翻炒10min，然后自然冷却至30～50摄氏度，于30～50摄氏度下低速离心，去沉淀，留液体，所述液体即为含石墨烯的鸡蛋油。
2.根据权利要求1所述的一种石墨烯润滑油，其特征在于，步骤2所述低速离心的转速为3000～5000转/分钟。
3.根据权利要求1所述的一种石墨烯润滑油，其特征在于，步骤1中所述氧化石墨烯采用少层氧化石墨烯。
4.根据权利要求1所述的一种石墨烯润滑油，其特征在于，所述助剂包括分散剂，黏度调节剂，抗泡剂，抗氧化剂，防锈剂中的一种或几种。
5.根据权利要求4所述的一种石墨烯润滑油，其特征在于，
所述分散剂为硬脂酸、十二烷基苯磺酸钠、脂肪酸甘油酯、三聚甘油单月桂酸酯、硬脂酸单甘油酯、季铵化物中的一种或几种；
所述黏度调节剂为聚甲基丙烯酸酯、烯烃共聚物中的一种或两种；
所述抗泡剂为烯甘油醚、二甲基硅油、乳化硅油和高碳醇脂肪酸酯复合物中的一种或几种；
所述抗氧化剂为双十二碳醇酯、三辛酯中的一种或两种；
所述防锈剂为石油磺酸钡、石油磺酸钠、二壬基萘磺酸钡、羊毛脂、蜂蜡、油酸十八烷胺和苯并三氮唑中的一种或几种。
6.根据权利要求5所述的一种石墨烯润滑油，其特征在于，所述烯烃共聚物采用氢化苯乙烯-双烯共聚物、乙丙共聚物中的一种或两种。
7.根据权利要求1所述的一种石墨烯润滑油，其特征在于，所述基础油为矿物油、聚α-烯烃、酯类油和聚醚类油中的一种或几种。
8.根据权利要求1所述的一种石墨烯润滑油，其特征在于，所述基础油采用液体石蜡。
9.一种如权利要求1～8任一项所述的石墨烯润滑油的制备方法，其特征在于，包括以下步骤：
按重量份称取各原料后，将含石墨烯的鸡蛋油和助剂加入到基础油中，采用高速搅拌机于100～120摄氏度、1200～1500转/分钟的转速下均质搅拌3～6小时至混合均匀，即得。
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