CN115109628B - 一种复合铝基润滑脂及其制备方法 - Google Patents

一种复合铝基润滑脂及其制备方法 Download PDF

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CN115109628B
CN115109628B CN202210805578.9A CN202210805578A CN115109628B CN 115109628 B CN115109628 B CN 115109628B CN 202210805578 A CN202210805578 A CN 202210805578A CN 115109628 B CN115109628 B CN 115109628B
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孙谦
贾展羽
梁雪蕊
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China Petroleum and Chemical Corp
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Abstract

本发明涉及润滑脂技术领域，具体涉及一种复合铝基润滑脂及其制备方法。该复合铝基润滑脂按重量份数计，包括以下组分：40～85份的基础油，5～15份的稠化剂，0.2～10份的石墨烯，0.1～0.3份的油溶性纳米氧化铈，所述稠化剂为复合铝基稠化剂。本发明提供的复合铝基润滑脂的质量稳定性好，具有优异的导电性、耐高温性、胶体安定性、机械安定性、化学安定性、抗磨性能和抗水性等综合性能。

Description

一种复合铝基润滑脂及其制备方法
技术领域
本发明涉及润滑脂技术领域，具体涉及一种复合铝基润滑脂及其制备方法。
背景技术
复合铝基润滑脂是用复合铝皂稠化基础油制备的。复合铝皂是一种由高碳酸、芳香酸与铝形成的碱式爽酸铝皂。早期的复合铝基润滑脂生产时采用复分解法生产，在声场碱式双酸铝皂，再经稠化基础油制备复合铝基润滑脂。这种方法生产复合铝皂的过程复杂，温度较高，不易控制制备的产品质量。目前生产复合铝基润滑脂主要采用铝的活性化合物直接与苯甲酸和脂肪酸进行皂化并分散在基础油中制备复合铝基润滑脂。这种方法简化了生产过程，生产易于操作，产品质量比较稳定，但仍存在抗磨性能较差，添加剂对环境有污染等问题。近年来，为了改善复合铝基润滑脂的性能，对其工艺流程，添加剂等方面做了大量的研究。纳米材料也逐渐用于润滑脂的应用中，如纳米二氧化硅、纳米金刚石等材料都开始进入润滑脂应用的相关研究之中。
发明内容
为了解决上述技术问题，本发明提供一种复合铝基润滑脂及其制备方法。
第一方面，本发明提供的复合铝基润滑脂，按重量份数计，包括以下组分：40～85份的基础油，5～15份的稠化剂，0.2～10份的石墨烯，0.1～0.3份的油溶性纳米氧化铈，所述稠化剂为复合铝基稠化剂。本发明提供的复合铝基润滑脂体系中石墨烯与复合铝基稠化剂能够增强皂分子固化基础油的能力，质量稳定性好且得到的复合铝基润滑脂产品导电性更佳，本发明加入了具有优良抗磨性的油溶性纳米氧化铈，减少了含有硫、磷等环境不友好元素的传统抗磨剂的使用，其环保性能大大增加。本发明通过配方各组分间相互作用，使得产品具有优异的导电性、耐高温性、胶体安定性、机械安定性、化学安定性、抗磨性能和抗水性等综合性能。
作为优选，包括以下组分：65～75份的基础油，10～15份的稠化剂，1～10份的石墨烯，0.1～0.2份的油溶性纳米氧化铈。
根据本发明的优选实施方式，在所述复合铝基润滑脂的制备过程中，所述石墨烯在皂化反应前加入，使得所述稠化剂依附于所述石墨烯周围，形成含石墨烯的胶团结构的复合铝基稠化剂。
本发明中石墨烯也可看作为稠化剂的一部分，即石墨烯在反应初期(皂化反应之前)加入到基础油中，与复合铝基稠化剂一起反应生成含有石墨烯的复合铝基润滑脂，能够显著提升润滑脂的导电性能及质量稳定性，同时结合油溶性纳米氧化铈，所得到的复合铝基润滑脂具有更好的导电性能及耐磨性等综合性能。
进一步优选，所述油溶性纳米氧化铈中的固体颗粒的粒径为30～80nm；优选的，按质量百分数计，所述油溶性纳米氧化铈的固含量为30～70％。本发明中，通过优化油溶性纳米氧化铈的粒径及固含量，能够进一步提高复合铝基润滑脂的抗磨性能。
进一步优选，所述石墨烯的粒径为80～800nm，电导率为700～900S/cm，分解温度为430～480℃。本发明中采用上述粒径、导电率和分解温度的石墨烯对于润滑脂的性能提升效果更明显。
进一步优选，所述稠化剂以硬脂酸、苯甲酸和异丙醇铝三聚体为原料制得，或以硬脂酸、对苯二甲酸和异丙醇铝三聚体为原料制得；优选的，所述异丙醇铝三聚体、硬脂酸与苯甲酸的质量比为4:1:1-4:9:1。
进一步优选，所述基础油的40℃运动粘度为90～100mm2/s，优选的，所述基础油选自矿物油、植物油、合成油或者它们的混合物；优选的40℃运动粘度为90-100mm2/s。植物油选自蓖麻油、花生油、菜籽油中的一种或多种，合成油选自是PAO、硅油、酯类油等中的一种或多种。所述基础油优选为500SN基础油、150BS基础油、650SN基础油或L-AN100基础油。
本发明中采用上述优选类型及参数的基础油和稠化剂的体系，能够更好发挥组分间的相互作用，使得润滑脂的综合性能得到显著提升。
第二方面，本发明提供的所述复合铝基润滑脂的制备方法，包括：将石墨烯、1/3～2/3基础油、硬脂酸、苯甲酸或对苯二甲酸、异丙醇铝三聚体混合，升温至80～100℃，进行皂化反应，升温，进行高温炼制，加入剩余的基础油，再加入油溶性纳米氧化铈，进行后处理。
本发明在反应前期将石墨烯加入作为稠化剂，这一做法使得稠化剂依附于其周围形成了类似胶团的结构，这种存在于石墨烯和皂分子之间的结构，存在一种协同作用，能够增强皂分子固化基础油的能力，极大地提升了成脂速度，缩短了皂化时间。本发明所提供的方式制备得到的复合铝基润滑脂产品质量稳定性好，在钢铁厂、汽车制造厂、尤其是火车气动刹车装置胜任润滑作用，且其能够更好地适用于高温潮湿条件下设备的润滑。
作为优选，包括：将石墨烯、1/3～2/3基础油、硬脂酸及苯甲酸混合，在搅拌下升温至80～85℃，待硬脂酸融化后，升温至90～100℃，加入异丙醇铝三聚体，进行皂化反应；升温至180～210℃、进行高温炼制；然后加入剩余的基础油冷却，待温度降至90℃以下加入油溶性纳米氧化铈，搅拌，分散，研磨。
进一步优选，所述皂化反应的温度为90～95℃，时间为1～1.5h。
进一步优选，所述高温炼制的温度为190～200℃，时间为10～20min。
本发明中，在上述优选制备工艺及温度参数下所得到的润滑脂综合性能更佳，尤其是通过对皂化反应条件和高温炼制条件进行优化能够使得润滑脂的调配效果更好。
本发明的有益效果至少在于：本发明提供的复合铝基润滑脂的制备方法操作简单，石墨烯在反应初期加入到基础油中，与复合铝基稠化剂一起反应生成含有石墨烯的复合铝基润滑脂，显著提高复合铝基润滑脂的导电性能，同时加入了油溶性纳米氧化铈的润滑脂具有降低的摩擦系数，减少了含有硫、磷等环境不友好元素的传统抗磨剂的使用，环保性能大大增加，配方各组分协同作用的润滑脂产品还具有优异的耐高温性，优良的胶体安定性、机械安定性、化学安定性、抗磨性能和抗水性等性能。本发明在反应前期将石墨烯加入作为稠化剂，能够极大地提升成脂速度，缩短皂化时间，制备得到的复合铝基润滑脂产品质量稳定性好，同时该脂可以在钢铁厂、汽车制造厂和火车气动刹车装置胜任润滑作用，尤其还适用于高温潮湿条件下设备的润滑。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述，以下实施例用于说明本发明，但不用来限制本发明的范围。实施例中未注明具体技术或条件者，按照本领域内的文献所描述的技术或条件，或者按照产品说明书进行。实施例中的实施条件可以根据具体的实验条件或者工厂条件进一步的调整，未注明实施条件的通常为常规实验中的条件。下述实施例中所用的材料、试剂等，如无特殊说明，均可从商业途径得到。
以下实施例用于说明本发明，但不用来限制本发明的范围。
本发明实施例中，所用油溶性纳米氧化铈的固体颗粒的粒径为60～65nm，按质量百分数计，所述油溶性纳米氧化铈的固含量为60～70％，溶剂为基础油。
本发明实施例中，所用石墨烯的粒径为600～800nm，电导率为800～850S/cm，分解温度为430～450℃。
实施例1
本实施例提供的复合铝基润滑脂，其配方组成为以下重量份的组分：500SN基础油(40℃运动粘度为100mm2/s)710份，石墨烯8份，12-羟基硬脂酸45份、苯甲酸5.12份、异丙醇铝三聚体19.63份，油溶性纳米氧化铈1份。
本实施例还提供该复合铝基润滑脂的制备方法：
将8克石墨烯、500克500SN基础油、45克12-羟基硬脂酸和5.12克苯甲酸加入反应釜中，搅拌加热升温至85℃，待硬脂酸溶解后，升温至95℃，加入19.63克异丙醇铝三聚体，进行皂化反应1小时。反应完全后升温至200℃，高温炼制10min。加入210克500SN基础油，待温度冷却到90℃，加入1克油溶性纳米氧化铈，充分搅拌，自然降温。最后经处理设备分散研磨后成品灌装。
实施例2
本实施例提供的复合铝基润滑脂，其配方组成为以下重量份的组分：
150BS基础油(40℃运动粘度为96mm2/s)420份，石墨烯60份，12-羟基硬脂酸37.96份、苯甲酸43.45份、异丙醇铝三聚体40.63份，油溶性纳米氧化铈2份。
本实施例还提供该复合铝基润滑脂的制备方法：
将60克石墨烯、200克150BS基础油、37.96克12-羟基硬脂酸和43.45克苯甲酸加入反应釜中，搅拌加热升温至84℃，待硬脂酸溶解后，升温至90℃，加入40.63克异丙醇铝三聚体，进行皂化反应1小时。反应完全后升温至195℃，高温炼制15min。加入220克150BS基础油，待温度冷却到90℃，加入2克油溶性纳米氧化铈，充分搅拌，自然降温。最后经处理设备分散研磨后成品灌装。
实施例3
本实施例提供的复合铝基润滑脂，其配方组成为以下重量份的组分：
650SN基础油(40℃运动粘度为120mm2/s)462份，石墨烯20份，12-羟基硬脂酸66.18份、对苯二甲酸40份、异丙醇铝三聚体46.63份，油溶性纳米氧化铈1.5份。
本实施例还提供该复合铝基润滑脂的制备方法：
将20克石墨烯、302克650SN基础油、66.18克12-羟基硬脂酸和40克对苯二甲酸加入反应釜中，搅拌加热升温至85℃，待硬脂酸溶解后，升温至95℃，加入46.63克异丙醇铝三聚体，进行皂化反应1小时。反应完全后升温至200℃，高温炼制10min。加入160克650SN基础油，待温度冷却到90℃，加入1.5克油溶性纳米氧化铈，充分搅拌，自然降温。最后经处理设备分散研磨后成品灌装。
实施例4
本实施例提供的复合铝基润滑脂，其配方组成为以下重量份的组分：
L-AN100基础油(40℃运动粘度为105mm2/s)670份，石墨烯40份，12-羟基硬脂酸68.32份、苯甲酸15.74份、异丙醇铝三聚体38.63份，油溶性纳米氧化铈1.8份。
本实施例还提供该复合铝基润滑脂的制备方法：
将40克石墨烯、500克L-AN100基础油、68.32克12-羟基硬脂酸和15.74克苯甲酸加入反应釜中，搅拌加热升温至85℃，待硬脂酸溶解后，升温至95℃，加入38.63克异丙醇铝三聚体，进行皂化反应1小时。反应完全后升温至195℃，高温炼制15min。加入170克基础油，待温度冷却到90℃，加入1.8克油溶性纳米氧化铈，充分搅拌，自然降温。最后经处理设备分散研磨后成品灌装。
对比例1
按照实施例1的方法制备复合铝基润滑脂，不同的是，复合铝基润滑脂的制备过程中不加入石墨烯。
对比例2
按照实施例1的方法制备复合铝基润滑脂，不同的是，复合铝基润滑脂的制备过程中不加入油溶性纳米氧化铈。
对实施例1～4和对比例1～2得到的润滑脂进行性能测试(测试结果见表1)。
表1润滑脂性能测试结果
从表1数据中可看出，本发明实施例1-4制备的复合铝基润滑脂均表现出优异耐高温、抗水性和粘附性、胶体安定性、极压抗磨性、防腐蚀性等性能，其中实施例4综合效果最佳。石墨烯的加入明显加快了反应的皂化时间，节约了反应时间。油溶性纳米氧化铈的加入明显改善了复合铝基润滑脂的抗摩擦性能，并且没有明显改变其本身所具有的特性，对其润滑性不会产生明显的负面影响，本发明的复合铝基润滑脂的质量稳定性好，具有优异的导电性、耐高温性、胶体安定性、机械安定性、化学安定性、抗磨性能和抗水性等综合性能。
虽然，上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述，但在本发明基础上，可以对之作一些修改或改进，这对本领域技术人员而言是显而易见的。因此，在不偏离本发明精神的基础上所做的这些修改或改进，均属于本发明要求保护的范围。

Claims (1)

1.一种复合铝基润滑脂的制备方法，其特征在于，采用以下重量份的组分：L-AN100基础油670份，40℃运动粘度为105mm2/s，石墨烯40份，12-羟基硬脂酸68.32份、苯甲酸15.74份、异丙醇铝三聚体38.63份，油溶性纳米氧化铈1.8份；所用油溶性纳米氧化铈的固体颗粒的粒径为60～65nm，按质量百分数计，所述油溶性纳米氧化铈的固含量为60～70％，溶剂为基础油；所用石墨烯的粒径为600～800nm，电导率为800～850S/cm，分解温度为430～450℃；
将40份石墨烯、500份L-AN100基础油、68.32份12-羟基硬脂酸和15.74份苯甲酸加入反应釜中，搅拌加热升温至85℃，待硬脂酸溶解后，升温至95℃，加入38.63份异丙醇铝三聚体，进行皂化反应1小时；反应完全后升温至195℃，高温炼制15min；加入170份L-AN100基础油，待温度冷却到90℃，加入1.8份油溶性纳米氧化铈，充分搅拌，自然降温；最后经处理设备分散研磨后成品灌装。
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