CN108559594B - 一种提高滴点和添加剂感受性的高性能复合锂基润滑脂及其制备工艺 - Google Patents
一种提高滴点和添加剂感受性的高性能复合锂基润滑脂及其制备工艺 Download PDFInfo
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Abstract
本发明公开了一种提高滴点和添加剂感受性的高性能复合锂基润滑脂及其制备工艺,所述高性能复合锂基润滑脂按重量份数计,包括以下组分:基础油307~325份,脂肪酸25~30份,二元有机酸12~15份,氢氧化锂12~16份,皂化水10~20份,桥联剂10~13份,急冷油85~93份,抗氧化剂0.8~1.5,有机减磨剂10~15份。本发明采用分级皂化工艺、分批加入原料以实现原料的充分混合与反应,在关键步骤中加入合适的桥联剂以解决润滑脂中油皂的作用力在高温条件下减弱、功能性添加剂分散不均、感受性不强等问题,从而提高润滑脂工作性能。
Description
技术领域
本发明涉及一种高性能复合锂基润滑脂及其制备方法,具体涉及一种提高滴点和添加剂感受性的高性能复合锂基润滑脂及其制备方法。
背景技术
在摩擦副之间使用润滑脂,使干摩擦转变为润滑脂分子内的摩擦,是减弱摩擦副间的磨损、减少能耗和保护器件的简易有效的方式。目前文献、专利报道有机类添加剂在润滑脂实际使用状况不稳定,而对润滑脂在高温作用下油皂分离、添加剂在润滑脂中如何实现较高的利用率鲜有报道。
发明内容
为了解决润滑脂在高温下容易滴油,添加剂在润滑脂中不易均匀分散且在润滑脂中感受性差的问题,本发明提供了一种提高滴点和添加剂感受性的高性能复合锂基润滑脂及其制备工艺。本发明采用分级皂化工艺、分批加入原料以实现原料的充分混合与反应,在关键步骤中加入合适的桥联剂以解决润滑脂中油皂的作用力在高温条件下减弱、功能性添加剂分散不均、感受性不强等问题,从而提高润滑脂工作性能。
本发明的目的是通过以下技术方案实现的:
一种提高滴点和添加剂感受性的高性能复合锂基润滑脂,按重量份数计,包括以下组分:基础油307~325份,脂肪酸25~30份,二元有机酸12~15份,氢氧化锂12~16份,皂化水10~20份,桥联剂10~13份,急冷油85~93份,抗氧化剂0.8~1.5,有机减磨剂10~15份。
一种上述高性能复合锂基润滑脂的制备工艺,如图1所示,包括如下步骤:
(1)一阶皂化:向反应釜中加入基础油205~220份、脂肪酸25~30份,升温至83~95℃,搅拌加热15~20min,搅拌速率为100~120r/min,使脂肪酸完全溶解;加入6~8份氢氧化锂、5~10份皂化水,升温至85~95℃,提高搅拌速率至120~145r/min,进行一阶皂化1~1.5h;
(2)二阶皂化:向反应釜中加入基础油32~40份、二元有机酸12~15份,升温至95~105℃,搅拌混合加热20~40min,搅拌速率230~300r/min,进行二阶皂化;
(3)三阶皂化:加入剩余的氢氧化锂和皂化水、10~13份桥联剂,升温至110~125℃,进行三阶皂化1.5~2.5h;
(4)脱水复合:皂化反应结束后,陆续升温至128~132℃、134~136℃,打开排水泵,脱去水分,各循环搅拌20~40min,进行脱水复合过程;
(5)高温复合:关闭排水泵,加入剩余基础油,升温至160~165℃,循环搅拌10~30min,使不同有机酸锂在桥联剂的作用下进一步复合;
(6)高温炼制:升温至180~185℃,加强皂纤维与基础油的混融程度,循环搅拌后,加入急冷油50~60份,开始降温;
(7)剪切冷却:降温至150~160℃,循环剪切,使析出的皂纤维均匀分布在体系内;
(8)冷却均化:降温至145~150℃,加入剩余急冷油,再加入抗氧化剂0.8~1.5份,循环剪切10~15min;
(9)研磨均化:将有机减磨剂10~15份加入研磨机中与复合锂基润滑脂混合均匀,即得复合锂基润滑脂。
本发明中,所述基础油可以为矿物润滑油、合成烃类、聚醚、聚硅氧烷、合成酯润滑油基础油中的两种及两种以上,或其中一种基础油的不同粘度的混合物。
本发明,所述脂肪酸种类包括C12-C17脂肪酸、12-羟基二十二烷酸、10-羟基棕榈酸等中的一种。
本发明中,所述二元有机酸包括壬二酸、癸二酸、丁二酸等中的一种。
本发明中,所述桥联剂包括壬二酸二甲酯、癸二酸二乙酯、癸二酸二丁酯、丁二酸二乙基己酯、己二酸二异辛酯、癸二酸二辛脂中的一种。
本发明,所述抗氧化剂包括2,6-二叔丁基对甲苯酚(BHT)、二苯胺及苯二胺类抗氧化剂等中的一种或几种的混合物。
本发明中,所述有机减磨剂主要包括二烷基二硫代磷酸锌(ZDDP)、二烷基二硫代磷酸钼(MoDDP)、二烷基二硫代甲酸钼(Mo-DTC)中的一种或几种的混合物。
相比于现有技术,本发明具有如下优点:
1、本发明通过探索润滑脂蒸发损失及油皂分离现象的原因,调整合成工艺并加入桥联剂,从而提供了一种既可以提高润滑脂滴点也可以提高添加剂在润滑脂感受性的合成工艺。
2、经摩擦相关测试分析,本发明制备出的润滑脂在苛刻环境中工作时,其添加剂表现出的性能较不经工艺改良的润滑脂的更好,能有效减弱摩擦副间的磨损,减少积温,抑制稠化剂和基础油的催化氧化,进而延长润滑脂的使用寿命和器件的服役时间。
附图说明
图1为本发明工艺流程图
图2为不同工艺制备出的润滑脂的摩擦系数随时间变化对比图;
图3为不同工艺制备出的润滑脂的平均摩擦系数对比图;
图4为不同工艺制备出的润滑脂的磨斑对比图,(a)1号样品,(b)2号样品,(c)3号样品。
具体实施方式
下面结合实施例对本发明的技术方案作进一步的说明,但并不局限于此,凡是对本发明技术方案进行修改或者等同替换,而不脱离本发明技术方案的精神和范围,均应涵盖在本发明的保护范围中。
实施例1:
本实施例中,提高滴点和添加剂感受性的高性能复合锂基润滑脂按重量份数计,包括以下组分:基础油(两种不同粘度的矿物润滑油400SN、150BS的混合物,二者质量比为1:1)310份、C12硬脂酸25份、癸二酸12份、氢氧化锂12份、皂化水14份、癸二酸二丁酯11份、二苯胺1.1份、急冷油89份、二烷基二硫代磷酸锌6份、二烷基二硫代甲酸钼4份。
上述高性能复合锂基润滑脂的制备步骤如下:
(1)一阶皂化:将215份基础油和25份C12硬脂酸加入开口反应釜中85℃加热搅拌30min,搅拌速率为110r/min,C12硬脂酸全部溶解后,加入6份氢氧化锂、7份皂化水,升温至95℃,提高搅拌速率至130r/min,反应1小时,进行一阶皂化。
(2)二阶皂化:向反应釜中加入12份癸二酸和35份基础油升温至100℃,反应30min,搅拌速率300r/min,进行二阶皂化。
(3)三阶皂化:加入剩余氢氧化锂和皂化水,11份癸二酸二丁酯,升温至120℃,反应2小时,进行三阶皂化反应。
(4)脱水复合:皂化反应结束后,相继升温至130℃、135℃各保温30分钟,打开排水泵,脱去水分,进行分段脱水复合过程;
(5)高温复合:关闭排水泵,加入剩余基础油,升温至165℃,循环搅拌20min,使两种锂皂进一步复合在一起。
(6)高温炼制:升温至185℃,使皂纤维与基础油和酯类合成油完全熔融后,加入54份急冷油,使皂纤维成形析出;
(7)剪切冷却:降温至160℃,冷却剪切30分钟,使皂纤维均匀分散在基础油中并形成三维网状结构;
(8)冷却均化:进一步降温至150℃,加入剩余急冷油和1.1份二苯胺,循环剪切15min;
(9)研磨均化:当温度降至50℃时,将预制好的混有添加剂的酯类合成油加入研磨机中,继续循环剪切,冷却,加入6份ZDDP和4份Mo-DTC研磨均化成脂。
实施例2:
本实施例中,提高滴点和添加剂感受性的高性能复合锂基润滑脂按重量份数计,包括以下组分:基础油(两种不同粘度的矿物润滑油400SN、150BS的混合物,二者质量比为1:1)320份、C12硬脂酸27份、癸二酸14份、氢氧化锂15份、皂化水20份、癸二酸二丁酯13份、二苯胺1.4份、急冷油86份、二烷基二硫代磷酸锌8份、二烷基二硫代甲酸钼4份。
上述高性能复合锂基润滑脂的制备步骤如下:
(1)一阶皂化:将220份部分基础油和27份C12硬脂酸加入开口反应釜中85℃加热搅拌15min,搅拌速率为110r/min,C12硬脂酸全部溶解后,加入7份氢氧化锂、10份皂化水,升温至95℃,提高搅拌速率至130r/min,反应1小时,进行一阶皂化。
(2)二阶皂化:向反应釜中加入14份癸二酸和40份基础油升温至100℃,反应30min,搅拌速率280r/min,进行二阶皂化。
(3)三阶皂化:加入剩余氢氧化锂和皂化水,13份癸二酸二丁酯,升温至120℃,反应2小时,进行三阶皂化反应。
(4)脱水复合:皂化反应结束后,相继升温至130℃、135℃各保温30分钟,打开排水泵,脱去水分,进行分段脱水复合过程;
(5)高温复合:关闭排水泵,加入剩余基础油,升温至165℃,循环搅拌20min,使两种锂皂进一步复合在一起。
(6)高温炼制:升温至185℃,使皂纤维与基础油和酯类合成油完全熔融后,加入58份急冷油,使皂纤维成形析出;
(7)剪切冷却:降温至160℃,冷却剪切30分钟,使皂纤维均匀分散在基础油中并形成三维网状结构;
(8)冷却均化:进一步降温至150℃,加入剩余急冷油和1.4份二苯胺,循环剪切15min;
(9)研磨均化:当温度降至50℃时,将预制好的混有添加剂的酯类合成油加入研磨机中,继续循环剪切,冷却,加入8份ZDDP和4份Mo-DTC研磨均化成脂。
润滑脂的滴点测试结果如表1所示,摩擦试验结果如图2-4所示,其中1号样品为未使用本发明合成工艺市售成品润滑脂,2、3号样品为按实施例1、2方法制备的复合锂基润滑脂。
表1 润滑脂滴点测试结果
润滑脂 | 1 | 2 | 3 |
滴点/℃ | 220.5 | 276.0 | 280.2 |
实施例3:
本实施例中,提高滴点和添加剂感受性的高性能复合锂基润滑脂按重量份数计,包括以下组分:基础油(聚醚和聚硅氧烷的混合物,二者质量比为1:1)315份、12-羟基二十二烷酸30份、丁二酸15份、氢氧化锂13份、皂化水12份、丁二酸二乙基己酯11份、2,6-二叔丁基对甲苯酚1.0份、急冷油92份、二烷基二硫代磷酸钼12份。
上述高性能复合锂基润滑脂的制备步骤如下:
(1)一阶皂化:将210份部分基础油和30份12-羟基二十二烷酸加入开口反应釜中85℃加热搅拌15min,搅拌速率为100r/min,12-羟基二十二烷酸全部溶解后,加入8份氢氧化锂、8份皂化水,升温至90℃,提高搅拌速率至140r/min,反应1小时,进行一阶皂化。
(2)二阶皂化:向反应釜中加入15份丁二酸和32份基础油升温至105℃,反应30min,搅拌速率250r/min,进行二阶皂化。
(3)三阶皂化:加入剩余氢氧化锂和皂化水,11份丁二酸二乙基己酯,升温至115℃,反应2小时,进行三阶皂化反应。
(4)脱水复合:皂化反应结束后,相继升温至130℃、135℃各保温30分钟,打开排水泵,脱去水分,进行分段脱水复合过程;
(5)高温复合:关闭排水泵,加入剩余基础油,升温至160℃,循环搅拌20min,使两种锂皂进一步复合在一起。
(6)高温炼制:升温至180℃,使皂纤维与基础油和酯类合成油完全熔融后,加入50份急冷油,使皂纤维成形析出;
(7)剪切冷却:降温至150℃,冷却剪切30分钟,使皂纤维均匀分散在基础油中并形成三维网状结构;
(7)剪切冷却:降温至150~160℃,循环剪切,使析出的皂纤维均匀分布在体系内;
(8)冷却均化:进一步降温至150℃,加入剩余急冷油和1.0份2,6-二叔丁基对甲苯酚,循环剪切10min;
(9)研磨均化:当温度降至50℃时,将预制好的混有添加剂的酯类合成油加入研磨机中,继续循环剪切,冷却,加入12份MoDDP研磨均化成脂。
Claims (5)
1.一种提高滴点和添加剂感受性的高性能复合锂基润滑脂,其特征在于所述高性能复合锂基润滑脂按重量份数计,包括以下原料:基础油307~325份,脂肪酸25~30份,二元有机酸12~15份,氢氧化锂12~16份,皂化水10~20份,桥联剂10~13份,急冷油85~93份,抗氧化剂0.8~1.5,有机减磨剂10~15份,所述脂肪酸种类为C12-C17脂肪酸、12-羟基二十二烷酸、10-羟基棕榈酸中的一种,二元有机酸为壬二酸、癸二酸、丁二酸中的一种,桥联剂为壬二酸二甲酯、癸二酸二乙酯、癸二酸二丁酯、丁二酸二乙基己酯、己二酸二异辛酯、癸二酸二辛酯中的一种,具体制备方法如下:
(1)一阶皂化:向反应釜中加入基础油205~220份、脂肪酸25~30份,升温至83~95℃,搅拌加热15~20min,搅拌速率为100~120r/min,使脂肪酸完全溶解;加入6~8份氢氧化锂、5~10份皂化水,升温至85~95℃,提高搅拌速率至120~145r/min,进行一阶皂化1~1.5h;
(2)二阶皂化:向反应釜中加入基础油32~40份、二元有机酸12~15份,升温至95~105℃,搅拌混合加热20~40min,搅拌速率230~300r/min,进行二阶皂化;
(3)三阶皂化:加入剩余的氢氧化锂和皂化水、10~13份桥联剂,升温至110~125℃,进行三阶皂化1.5~2.5h;
(4)脱水复合:皂化反应结束后,陆续升温至128~132℃、134~136℃,打开排水泵,脱去水分,各循环搅拌20~40min,进行脱水复合过程;
(5)高温复合:关闭排水泵,加入剩余基础油,升温至160~165℃,循环搅拌10~30min,使不同有机酸锂在桥联剂的作用下进一步复合;
(6)高温炼制:升温至180~185℃,加强皂纤维与基础油的混融程度,循环搅拌后,加入急冷油50~60份,开始降温;
(7)剪切冷却:降温至150~160℃,循环剪切,使析出的皂纤维均匀分布在体系内;
(8)冷却均化:降温至145~150℃,加入剩余急冷油,再加入抗氧化剂0.8~1.5份,循环剪切10~15min;
(9)研磨均化:将有机减磨剂10~15份加入研磨机中与复合锂基润滑脂混合均匀,即得复合锂基润滑脂。
2.根据权利要求1所述的提高滴点和添加剂感受性的高性能复合锂基润滑脂,其特征在于所述基础油为矿物润滑油、合成烃类、聚醚、聚硅氧烷、合成酯润滑油基础油中的两种及两种以上,或其中一种基础油的不同粘度的混合物。
3.根据权利要求1所述的提高滴点和添加剂感受性的高性能复合锂基润滑脂,其特征在于所述抗氧化剂为2,6-二叔丁基对甲苯酚、二苯胺及苯二胺类抗氧化剂中的一种或几种的混合物。
4.根据权利要求1所述的提高滴点和添加剂感受性的高性能复合锂基润滑脂,其特征在于所述有机减磨剂为二烷基二硫代磷酸锌、二烷基二硫代磷酸钼、二烷基二硫代甲酸钼中的一种或几种的混合物。
5.一种权利要求1-4任一权利要求所述的高性能复合锂基润滑脂的制备工艺,其特征在于所述工艺步骤如下:
(1)一阶皂化:向反应釜中加入基础油205~220份、脂肪酸25~30份,升温至83~95℃,搅拌加热15~20min,搅拌速率为100~120r/min,使脂肪酸完全溶解;加入6~8份氢氧化锂、5~10份皂化水,升温至85~95℃,提高搅拌速率至120~145r/min,进行一阶皂化1~1.5h;
(2)二阶皂化:向反应釜中加入基础油32~40份、二元有机酸12~15份,升温至95~105℃,搅拌混合加热20~40min,搅拌速率230~300r/min,进行二阶皂化;
(3)三阶皂化:加入剩余的氢氧化锂和皂化水、10~13份桥联剂,升温至110~125℃,进行三阶皂化1.5~2.5h;
(4)脱水复合:皂化反应结束后,陆续升温至128~132℃、134~136℃,打开排水泵,脱去水分,各循环搅拌20~40min,进行脱水复合过程;
(5)高温复合:关闭排水泵,加入剩余基础油,升温至160~165℃,循环搅拌10~30min,使不同有机酸锂在桥联剂的作用下进一步复合;
(6)高温炼制:升温至180~185℃,加强皂纤维与基础油的混融程度,循环搅拌后,加入急冷油50~60份,开始降温;
(7)剪切冷却:降温至150~160℃,循环剪切,使析出的皂纤维均匀分布在体系内;
(8)冷却均化:降温至145~150℃,加入剩余急冷油,再加入抗氧化剂0.8~1.5份,循环剪切10~15min;
(9)研磨均化:将有机减磨剂10~15份加入研磨机中与复合锂基润滑脂混合均匀,即得复合锂基润滑脂。
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