CN106381192B - 一种石墨烯液压油的制备方法 - Google Patents

一种石墨烯液压油的制备方法 Download PDF

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CN106381192B
CN106381192B CN201610740084.1A CN201610740084A CN106381192B CN 106381192 B CN106381192 B CN 106381192B CN 201610740084 A CN201610740084 A CN 201610740084A CN 106381192 B CN106381192 B CN 106381192B
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CN106381192A (zh
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吴美燕
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Zibo Huihua Petroleum Additives Co., Ltd.
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Abstract

本发明涉及一种石墨烯液压油的制备方法，将消泡剂、分散剂加入到煤油中，搅拌均匀后，在高速剪切的状态下加入石墨烯和粉料，使石墨烯、粉料和热稳定剂完全分散于煤油中后，加入抗氧剂、基础油和蜡，在一定压力、温度、高速剪切状态下蒸馏一定时间，冷却回收蒸馏出的煤油，蒸馏后的产物即为石墨烯液压油。该产品通过石墨烯的加入，可以提高液压油对所保护部件的抗磨性能，还可以提高液压油的抗热性能。

Description

一种石墨烯液压油的制备方法
技术领域
本发明涉及一种石墨烯液压油的制备方法。
背景技术
液压油在使用过程中可能因环境潮湿而导致进水，破坏油的乳化平衡导致制动、转向液压系统温度升高、液压油内泄，从而使液压油消耗增大并使其耐磨能力下降。
发明内容
本发明所要解决的技术问题是，提供一种石墨烯液压油的制备方法，制备的产品热稳定性好，并具有优异的抗摩擦和密封性能。
为了解决上述技术问题，本发明采用了以下技术方案：
一种石墨烯液压油的制备方法，其特征在于按照以下步骤进行：
1）制备产品A：将消泡剂、分散剂和煤油按照质量比0.5～3:0.5～3:1000加入到高剪切设备中，搅拌均匀，得到产品A；
2）制备产品B：在高速剪切的状态下将石墨烯、粉料和热稳定剂分别加入到产品A中，得到产品B，石墨烯、粉料、热稳定剂和产品A的质量比为0.5～4:10～40:1～10:60～90；
3）制备产品C：将基础油、抗氧剂和蜡分别加入到产品B中，搅拌至蜡完全溶解，得到产品C，基础油、抗氧剂、蜡和产品B的质量比为58～88:1～10:1～5:10～40；
4）制备石墨烯液压油：在压力为-0.1MPa～-1.5MPa，温度为60℃～120℃，对产品C搅拌蒸馏15min～60min，冷却回收蒸馏出的煤油，向蒸馏出煤油的产物中加入消泡剂，,搅拌均匀后即得到石墨烯液压油消泡剂和蒸馏出煤油的产物的质量比为0.5～5:1000；
所述消泡剂是斯盘-80、二甲基硅油、油性非硅类消泡剂DF-520和油性非硅类消泡剂DF-530中的一种或任意比例的两种以上；
所述分散剂是三乙基己基磷酸、双烯基丁二酰亚胺T154、乙烯基双硬脂酰胺、硬脂酸单甘油酯、聚乙二醇和单烯基丁二酰亚胺中的一种或任意比例的两种以上；
所述粉料为二氧化硅、滑石粉和高岭土中的一种或任意比例的两种以上；
所述热稳定剂是Ca-Zn复合热稳定剂、二盐基硬脂酸铅稳定剂和二盐基亚磷酸铅中的一种或任意比例的两种以上；
所述抗氧剂是2，6-三级丁基-4-甲基苯酚、双（3，5-三级丁基-4-羟基苯基）硫醚、四〔β-(3，5-三级丁基-4-羟基苯基)丙酸〕季戊四醇酯、双十二碳醇酯、双十四碳醇酯和双十八碳醇酯中的一种或任意比例的两种以上；
所述蜡为石蜡、微晶蜡、醋酸乙烯共聚蜡、硬脂酸锌和蜂蜡中的一种或任意比例的两种以上。
所述高速剪切的转速为1000转/min～5000转/min。
步骤1）中消泡剂为油性非硅类消泡剂DF-520；分散剂为双烯基丁二酰亚胺T154和乙烯基双硬脂酰胺按照质量比3:1的组合物；消泡剂、分散剂和煤油的质量比为1.5:1:1000。
步骤2）中高速剪切转速为3000转/min；粉料为二氧化硅和滑石粉按照质量比5:1的组合物；热稳定剂是Ca-Zn复合热稳定剂；石墨烯、粉料、热稳定剂和产品A的质量比为4:16:2:78。
步骤3）中蜡为85#微晶蜡、醋酸乙烯共聚蜡和硬脂酸锌按照质量比2:5:1的组合物；抗氧剂为2，6-三级丁基-4-甲基苯酚、双（3，5-三级丁基-4-羟基苯基）硫醚和双十二碳醇酯按照质量比2:1:1的组合物；基础油、抗氧剂、蜡和产品B的质量比为78:3:2:17。
步骤4）中压力为-1.2MPa，温度为85℃，蒸馏时间为40min；消泡剂为斯盘-80和二甲基硅油按照质量比1:1的组合物；消泡剂和蒸馏出煤油的产物的质量比为1.5:1000。
本发明具有以下有益技术效果：
1）、本发明采用煤油做分散溶剂，主要因为煤油具有较低的粘性，物料在煤油中更容易分散，分散效果好，直接以基础油为分散溶剂，基础油粘性要比煤油大的多，分散效果不好，影响产品效果。
2）、本发明通过物理和化学的方法将石墨烯和粉料稳定分散悬浮于液压油中，不会絮凝和沉积。
3）、本发明石墨烯和抗氧剂的加入可以增加液压油的抗热性能和液压油的抗氧化性能，使用更长久。
4）、本发明采用85#微晶蜡、醋酸乙烯共聚蜡和硬脂酸锌为成膜材料，具有韧性好、附着力强的优点，不会因使用密封材料脆产生裂纹导致水的进入，破坏液压油的乳化稳定性。
5）、本发明加入Ca-Zn复合热稳定剂使液压油在热的条件下稳定。
6）、本发明使用时，可以形成超强油膜粘附在金属表面，形成类似抛光的“油镀”，石墨烯优异的弹性性能，可以对部件之间的摩擦产生缓冲，更好的对部件进行保护。
7）、本发明选用石墨烯作为改性剂，与稀土氟化物相比环保性能更高。
8）、本发明将低分子量的煤油蒸馏出来，可以防止液压油发热时，煤油蒸发落于设备某些部位，长期积累煤油降解对设备造成腐蚀。
9）、本发明在煤油蒸馏后加入消泡剂，防止液压油在使用时产生气泡，气泡破裂导致密封性不好而进水，破坏油的乳化平衡。
具体实施方式
下面结合具体实例进一步说明本发明。
实施例一
将消泡剂、分散剂和煤油按照质量比1.5:1:1000加入到高剪切设备中，搅拌均匀，得到产品A；在3000转/min高速剪切的状态下，将石墨烯、粉料和热稳定剂按照一定质量比加入到产品A中，石墨烯、粉料、热稳定剂和产品A的质量比为4:16:2:78，得到产品B；将基础油、抗氧剂和蜡按照一定质量比加入到产品B中，基础油、抗氧剂、蜡和产品B的质量比为78:3:2:17，搅拌至蜡完全溶解，在压力为-1.2MPa，温度为85℃，搅拌蒸馏40min，冷却回收蒸馏出的煤油，向蒸馏出煤油的产物中加入一定质量比的消泡剂，消泡剂和蒸馏出煤油的产物的质量比为1.5:1000,即得到石墨烯液压油。
实施例二
将消泡剂、分散剂和煤油按照质量比1.5:1:1000加入到高剪切设备中，搅拌均匀，得到产品A；在3000转/min高速剪切的状态下，将石墨烯、粉料和热稳定剂按照一定质量比加入到产品A中，石墨烯、粉料、热稳定剂和产品A的质量比为4:16:2:78，得到产品B；将基础油、抗氧剂和蜡按照一定质量比加入到产品B中，基础油、抗氧剂、蜡和产品B的质量比为78:3:2:17，搅拌至蜡完全溶解，在压力为-1.2MPa，温度为85℃，搅拌蒸馏40min，冷却回收蒸馏出的煤油，向蒸馏出煤油的产物中加入一定质量比的消泡剂，消泡剂和蒸馏出煤油的产物的质量比为0.5:1000,即得到石墨烯液压油。
实施例三
将消泡剂、分散剂和煤油按照质量比1.5:1:1000加入到高剪切设备中，搅拌均匀，得到产品A；在3000转/min高速剪切的状态下，将石墨烯、粉料和热稳定剂按照一定质量比加入到产品A中，石墨烯、粉料、热稳定剂和产品A的质量比为4:16:2:78，得到产品B；将基础油、抗氧剂和蜡按照一定质量比加入到产品B中，基础油、抗氧剂、蜡和产品B的质量比为78:3:2:17，搅拌至蜡完全溶解，在压力为-1.2MPa，温度为85℃，搅拌蒸馏40min，冷却回收蒸馏出的煤油，向蒸馏出煤油的产物中加入一定质量比的消泡剂，消泡剂和蒸馏出煤油的产物的质量比为1:1000,即得到石墨烯液压油。
实施例四
将消泡剂、分散剂和煤油按照质量比1.5:1:1000加入到高剪切设备中，搅拌均匀，得到产品A；在3000转/min高速剪切的状态下，将石墨烯、粉料和热稳定剂按照一定质量比加入到产品A中，石墨烯、粉料、热稳定剂和产品A的质量比为4:16:2:78，得到产品B；将基础油、抗氧剂和蜡按照一定质量比加入到产品B中，基础油、抗氧剂、蜡和产品B的质量比为78:3:2:17，搅拌至蜡完全溶解，在压力为-1.2MPa，温度为85℃，搅拌蒸馏40min，冷却回收蒸馏出的煤油，向蒸馏出煤油的产物中加入一定质量比的消泡剂，消泡剂和蒸馏出煤油的产物的质量比为2:1000,即得到石墨烯液压油。
实施例1至4中消泡剂是油性非硅类消泡剂DF-520；分散剂为双烯基丁二酰亚胺T154和乙烯基双硬脂酰胺按照质量比3:1的组合物；粉料为二氧化硅和滑石粉按照质量比5:1的组合物；热稳定剂是Ca-Zn复合热稳定剂；蜡为85#微晶蜡、醋酸乙烯共聚蜡和硬脂酸锌按照质量比2:5:1的组合物；抗氧剂为2，6-三级丁基-4-甲基苯酚、双（3，5-三级丁基-4-羟基苯基）硫醚和双十二碳醇酯按照质量比2:1:1的组合物。
下面结合实验数据进一步说明本发明的有益效果：
1、实验供试材料
1材料与方法：
1.1供试材料：本发明实施例1、实施例2、实施例3、实施例4和普通液压油（除蒸馏出煤油后未加消泡剂外，其它制作方法均与实施例1相同）做效果比较。
1.2试验设计：试验设5个处理，做平行。取同样质量的实施例1、实施例2、实施例3、实施例4和普通液压油（除蒸馏出煤油后未加消泡剂外，其它制作方法均与实施例1相同）分别均匀涂抹于矿车的叶片泵、柱塞泵和齿轮泵液压系统上，工作3个月后做第一次维护，观察叶片泵、柱塞泵和齿轮泵液压系统上润滑油情况及磨损情况。
本实验除采用的处理不同外其他条件均一致。
2结果与分析
其中普通液压油（除蒸馏出煤油后未加消泡剂外，其它制作方法均与实施例1相同），在使用两个月时，液压油因进水，液压油损耗严重，工作人员对液压油做了清洗并更换，而使用本发明制备的实施例1至4液压油完好。使用三个月第一次维护时，发现实施例2和实施例3液压油表面有坑凹，且损耗较大作人员对液压油做了清洗并更换，而实施例1和实施例4液压油表面未有坑凹现象，损耗少未做更换。
实施例1、实施例2、实施例3、实施例4和普通液压油（除蒸馏出煤油后未加消泡剂外，其它制作方法均与实施例1相同）处理相比，结果如表1。
表1 各处理对叶片泵、活塞泵和齿轮泵磨损情况的影响
叶片泵（%） 活塞泵（%） 齿轮泵（%）
实施例1 未发现磨损 未发现磨损 未发现磨损
实施例2 有磨损不明显 有磨损不明显 有磨损不明显
实施例3 有磨损不明显 有磨损不明显 有磨损不明显
实施例4 未发现磨损 未发现磨损 未发现磨损
普通液压油 有磨损，肉眼可以看到 有磨损，肉眼可以看到 有磨损，肉眼可以看到
由表1可以使用本发明制备的实施例1至4无论是在抗磨损还是在使用寿命方面效果优于普通液压油。实施例2和实施例3可能因为消泡剂的量不够，导致在热的环境下使用时，产生气泡并且气泡破裂，导致表面坑凹，且损耗严重，实施例1和实施例4虽然都使用效果不错，但从经济学角度实施例1效果最好。

Claims (6)

1.一种石墨烯液压油的制备方法，其特征在于按照以下步骤进行：
1）制备产品A：将消泡剂、分散剂和煤油按照质量比0.5～3:0.5～3:1000加入到高剪切设备中，搅拌均匀，得到产品A；
2）制备产品B：在高速剪切的状态下将石墨烯、粉料和热稳定剂分别加入到产品A中，得到产品B，石墨烯、粉料、热稳定剂和产品A的质量比为0.5～4:10～40:1～10:60～90；
3）制备产品C：将基础油、抗氧剂和蜡分别加入到产品B中，搅拌至蜡完全溶解，得到产品C，基础油、抗氧剂、蜡和产品B的质量比为58～88:1～10:1～5:10～40；
4）制备石墨烯液压油：在压力为-0.1MPa～-1.5MPa，温度为60℃～120℃，对产品C搅拌蒸馏15min～60min，冷却回收蒸馏出的煤油，向蒸馏出煤油的产物中加入消泡剂，搅拌均匀后即得到石墨烯液压油， 消泡剂和蒸馏出煤油的产物的质量比为0.5～5:1000；
所述消泡剂是斯盘-80、二甲基硅油、油性非硅类消泡剂DF-520和油性非硅类消泡剂DF-530中的一种或任意比例的两种以上；
所述分散剂是三乙基己基磷酸、双烯基丁二酰亚胺T154、乙烯基双硬脂酰胺、硬脂酸单甘油酯、聚乙二醇和单烯基丁二酰亚胺中的一种或任意比例的两种以上；
所述粉料为二氧化硅、滑石粉和高岭土中的一种或任意比例的两种以上；
所述热稳定剂是Ca-Zn复合热稳定剂、二盐基硬脂酸铅稳定剂和二盐基亚磷酸铅中的一种或任意比例的两种以上；
所述抗氧剂是2，6-三级丁基-4-甲基苯酚、双（3，5-三级丁基-4-羟基苯基）硫醚、四〔β-(3，5-三级丁基-4-羟基苯基)丙酸〕季戊四醇酯、双十二碳醇酯、双十四碳醇酯和双十八碳醇酯中的一种或任意比例的两种以上；
所述蜡为石蜡、微晶蜡、醋酸乙烯共聚蜡、硬脂酸锌和蜂蜡中的一种或任意比例的两种以上。
2.如权利要求1所述的石墨烯液压油的制备方法，其特征在于：所述高速剪切的转速为1000转/min～5000转/min。
3.如权利要求1所述的石墨烯液压油的制备方法，其特征在于：步骤1）中消泡剂为油性非硅类消泡剂DF-520；分散剂为双烯基丁二酰亚胺T154和乙烯基双硬脂酰胺按照质量比3:1的组合物；消泡剂、分散剂和煤油的质量比为1.5:1:1000。
4.如权利要求1所述的石墨烯液压油的制备方法，其特征在于：步骤2）中高速剪切转速为3000转/min；粉料为二氧化硅和滑石粉按照质量比5:1的组合物；热稳定剂是Ca-Zn复合热稳定剂；石墨烯、粉料、热稳定剂和产品A的质量比为4:16:2:78。
5.如权利要求1所述的石墨烯液压油的制备方法，其特征在于：步骤3）中蜡为85#微晶蜡、醋酸乙烯共聚蜡和硬脂酸锌按照质量比2:5:1的组合物；抗氧剂为2，6-三级丁基-4-甲基苯酚、双（3，5-三级丁基-4-羟基苯基）硫醚和双十二碳醇酯按照质量比2:1:1的组合物；基础油、抗氧剂、蜡和产品B的质量比为78:3:2:17。
6.如权利要求1所述的石墨烯液压油的制备方法，其特征在于：步骤4）中压力为-1.2MPa，温度为85℃，蒸馏时间为40min；消泡剂为斯盘-80和二甲基硅油按照质量比1:1的组合物；消泡剂和蒸馏出煤油的产物的质量比为1.5:1000。
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