CN111205909B - 一种复合锂基润滑脂及其制备方法 - Google Patents

一种复合锂基润滑脂及其制备方法 Download PDF

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CN111205909B
CN111205909B CN201811405004.2A CN201811405004A CN111205909B CN 111205909 B CN111205909 B CN 111205909B CN 201811405004 A CN201811405004 A CN 201811405004A CN 111205909 B CN111205909 B CN 111205909B
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邱辉玉
王春耕
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Beijing Shengxin Hexie Lubricating Grease Co ltd
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Abstract

本发明公开了一种复合锂基润滑脂，由以下重量份的原料制成：70~85份矿物油、7.5~15份脂肪酸、1.8~3份氢氧化锂、0.1~0.25份氢氧化钙、0.2~0.6份抗氧剂、2~7.5份极压剂、0.05~0.2份防锈剂和2~6份增稠剂。本发明还公开了一种复合锂基润滑脂的制备方法，包括以下步骤：S1：将650SN和150BS混合搅拌，升温至80~100℃，加水7~13份，然后加入氢氧化锂和氢氧化钙和脂肪酸，在120~130℃下皂化反应1~2h；S2：升温至130~145℃，脱水60~90min，升温至160~170℃时，加入抗氧剂，然后继续升温至210~220℃，高温炼制10~30min；S3：加入剩余的1/3矿物油，并急速降温至145~175℃，在0.8~1.0MPa下剪切2~2.5h；S4：降温至90~100℃，加入增稠剂、极压剂和防锈剂，搅拌均匀后，均质，过滤。本发明的优点是制得的润滑脂具有优异的极压抗磨性能。

Description

一种复合锂基润滑脂及其制备方法
技术领域
本发明涉及润滑脂领域，更具体地说，它涉及一种复合锂基润滑脂及其制备方法。
背景技术
复合锂基润滑脂是由羟基脂肪酸锂皂与低分子酸锂盐复合生成的复合锂皂稠化基础油并加入添加剂制备的润滑脂，具有更高的滴点及高温性能，广泛地应用于钢铁、汽车等行业。然而，由于受到脂皂结构和添加剂的所限，大都存在润滑脂进水后的极压性能大幅下降的情况，由此造成设备运行过程中，轴承缺少润滑而造成磨损，出现润滑故障，影响正常生产。
发明内容
针对现有技术存在的不足，本发明的第一个目的在于提供一种复合锂基润滑脂，其具有更高极压抗磨性能的优点。
本发明的第二个目的在于提供一种复合锂基润滑脂的制备方法，其具有制得的润滑油具有更高的极压耐磨性能的优点。
为实现上述第一个目的，本发明提供了如下技术方案：一种复合锂基润滑脂，由以下重量份的原料制成：70～85份矿物油、7.5～15份脂肪酸、1.8～3份氢氧化锂、0.1～0.25份氢氧化钙、0.2～0.6份抗氧剂、2～7.5份极压剂、0.05～0.2份防锈剂和2～6份增稠剂。
通过采用上述技术方案，极压剂的加入使得制得的复合锂基润滑脂的极压性能良好，尤其是硫代磷酸三苯酯、辛基丁基二苯胺、磷酸铵和氨基代酯几种润滑脂的复配，制得的润滑脂具有优异的极压抗磨能，大大降低在使用时轴承缺少润滑而影响工作的几率，特别适用于工况条件复杂的情况。
进一步地，该复合锂基润滑脂由以下重量份的原料制成：75～85份矿物油、9～12份脂肪酸、1.8～2.5份氢氧化锂、0.1～0.25份氢氧化钙、0.2～0.5份抗氧剂、4～6份极压剂、0.05～0.15份防锈剂和2～4份增稠剂。
进一步地，该复合锂基润滑脂由以下重量份的原料制成：80份矿物油、10份脂肪酸、2份氢氧化锂、0.2份氢氧化钙、0.3份抗氧剂、5份极压剂、0.1份防锈剂和2.4份增稠剂。
进一步地，所述矿物油包括60％～80％的650SN，余量为150BS，该矿物油100℃的运动粘度为14～16mm2/s。
进一步地，所述极压剂为硫代磷酸三苯酯、辛基丁基二苯胺、磷酸铵和氨基硫代酯中的一种或几种。
进一步地，所述抗氧剂为二苯胺与苯三唑衍生物其中的一种或两者以任意比例复配。
进一步地，所述的防锈剂为：苯并三氮唑与噻二唑衍生物中的一种或两者以任意比例复配。
进一步地，所述增稠剂为聚异丁烯与乙丙共聚物的一种或两者以任意比例复配；
所述脂肪酸为12-羟基硬脂酸与癸二酸的一种或两者以任意比例复配。
为实现上述第二个目的，本发明提供了如下技术方案：一种复合锂基润滑脂的制备方法，包括以下步骤：
S1：将650SN和150BS混合搅拌，升温至80～100℃，加水7～13重量份，然后加入氢氧化锂和氢氧化钙，搅拌3～10min后加入脂肪酸，在120～130℃下皂化反应1～2h；
S2：升温至130～145℃，脱水60～90min，升温至160～170℃时，加入抗氧剂，然后继续升温至210～220℃，高温炼制10～30min；
S3：加入剩余的1/3矿物油，并急速降温至145～175℃，在0.8～1.0MPa下剪切2～2.5h；
S4：降温至90～100℃，加入增稠剂、极压剂和防锈剂，搅拌均匀后，均质，过滤后即得复合锂基润滑脂。
进一步地，步骤S1中氢氧化钙以悬浊液的方式加入，即氢氧化钙与水以1:10～20混合后加入。
综上所述，本发明具有以下有益效果：
采用极压剂，尤其是硫代磷酸三苯酯、辛基丁基二苯胺、磷酸铵和氨基代酯几种润滑脂的复配，制得的润滑脂具有优异的极压抗磨能，大大降低在使用时轴承缺少润滑而影响工作的几率，特别适用于工况条件复杂的情况。
具体实施方式
以下结合实施例对本发明作进一步详细说明。
一种复合锂基润滑脂，由以下重量份的原料制成：70～85份矿物油、7.5～15份脂肪酸、1.8～3份氢氧化锂、0.1～0.25份氢氧化钙、0.2～0.6份抗氧剂、2～7.5份极压剂、0.05～0.2份防锈剂和2～6份增稠剂。
其中，矿物油包括60％～80％的650SN，余量为150BS，该矿物油100℃的运动粘度为14～16mm2/s；
极压剂为硫代磷酸三苯酯、辛基丁基二苯胺、磷酸铵和氨基硫代酯中的一种或几种；
抗氧剂为二苯胺与苯三唑衍生物其中的一种或两者以任意比例复配；
防锈剂为：苯并三氮唑与噻二唑衍生物中的一种或两者以任意比例复配；
增稠剂为聚异丁烯与乙丙共聚物的一种或两者以任意比例复配；
脂肪酸为12-羟基硬脂酸与癸二酸的一种或两者以任意比例复配。
以下实施例中的原料均可市售得到。
实施例1
一种复合锂基润滑脂，以重量份数计，通过以下步骤制得：
S1：将44份650SN和10份150BS投入反应釜，搅拌升温至90℃，然后加水8份，加入2份氢氧化锂和0.2份氢氧化钙，搅拌5min后，投入全部的3份癸二酸与7份12-羟基硬脂酸在125℃下皂化反应1.5h；
S2：升温至140℃，脱水90分钟，继续升温至170℃，加入0.3份二苯胺，然后继续升温至215℃，高温炼制15分钟；
S3：加入21份650SN和5份150BS，并急速降温至160℃，在0.8MPa下剪切2h；
S4：降温至90℃，加入2.4份聚异丁烯、0.5份辛基丁基二苯胺、2份磷酸胺、2份氨基硫代酯、0.5份硫代磷酸三苯酯和0.1份苯并三氮唑，搅拌均匀后，均质，过滤后即得复合锂基润滑脂。
实施例2～17按照实施例1中的方法进行，不同之处在于，添加的原料以及用量按照表1进行。
表1：
Figure BDA0001876352190000031
Figure BDA0001876352190000041
实施例18
一种复合锂基润滑脂，以重量份数计，通过以下步骤制得：
S1：将44份650SN和10份150BS投入反应釜，搅拌升温至80℃，然后加水7份，加入2份氢氧化锂和0.2份氢氧化钙，搅拌3min后，投入全部的3份癸二酸与7份12-羟基硬脂酸，在120℃下皂化反应1h；
S2：升温至130℃，脱水60分钟，继续升温至160℃，加入0.3份二苯胺，然后继续升温至210℃，高温炼制10分钟；
S3：加入21份650SN和5份150BS，并急速降温至145℃，在0.8MPa下剪切2h；
S4：降温至90℃，加入2.4份聚异丁烯、0.5份辛基丁基二苯胺、2份磷酸胺、2份氨基硫代酯、0.5份硫代磷酸三苯酯和0.1份苯并三氮唑，搅拌均匀后，均质，过滤后即得复合锂基润滑脂。
实施例19
一种复合锂基润滑脂，以重量份数计，通过以下步骤制得：
S1：将44份650SN和10份150BS投入反应釜，搅拌升温至90℃，然后加水13重量份，加入2份氢氧化锂和0.2份氢氧化钙，搅拌6min后，投入全部的3份癸二酸与7份12-羟基硬脂酸，在125℃下皂化反应1.5h；
S2：升温至140℃，脱水75分钟，继续升温至165℃，加入0.3份二苯胺，然后继续升温至215℃，高温炼制15分钟；
S3：加入21份650SN和5份150BS，并急速降温至160℃，在0.9MPa下剪切2.2h；
S4：降温至95℃，加入2.4份聚异丁烯、0.5份辛基丁基二苯胺、2份磷酸胺、2份氨基硫代酯、0.5份硫代磷酸三苯酯和0.1份苯并三氮唑，搅拌均匀后，均质，过滤后即得复合锂基润滑脂。
实施例20
一种复合锂基润滑脂，以重量份数计，通过以下步骤制得：
S1：将44份650SN和10份150BS投入反应釜，搅拌升温至100℃，然后加水10重量份，加入2份氢氧化锂和0.2份氢氧化钙，搅拌10min后，投入全部的3份癸二酸与7份12-羟基硬脂酸，在130℃下皂化反应2h；
S2：升温至145℃，脱水90分钟，继续升温至170℃，加入0.3份二苯胺，然后继续升温至220℃，高温炼制30分钟；
S3：加入21份650SN和5份150BS，并急速降温至175℃，在1.0MPa下剪切2.5h；
S4：降温至100℃，加入2.4份聚异丁烯、0.5份辛基丁基二苯胺、2份磷酸胺、2份氨基硫代酯、0.5份硫代磷酸三苯酯和0.1份苯并三氮唑，搅拌均匀后，均质，过滤后即得复合锂基润滑脂。
实施例21
按照实施例1的方法进行，不同之处在于，氢氧化钙以悬浊液的方式加入，即氢氧化钙与水以1：10混合后加入。
实施例22
按照实施例1的方法进行，不同之处在于，氢氧化钙以悬浊液的方式加入，即氢氧化钙与水以1：20混合后加入。
实施例23
按照实施例1的方法进行，不同之处在于，氢氧化钙以悬浊液的方式加入，即氢氧化钙与水以1：15混合后加入。
性能检测
对以上实施例进行滴点、钢网分油、极压性能、抗磨性能及耐水性能检测，检测结果见表2。
表2：
Figure BDA0001876352190000051
Figure BDA0001876352190000061
Figure BDA0001876352190000071
由上表可知，本发明制得的复合锂基润滑脂具有优异的极压抗磨性。
本具体实施例仅仅是对本发明的解释，其并不是对本发明的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改，但只要在本发明的权利要求范围内都受到专利法的保护。

Claims (2)

1.一种复合锂基润滑脂的制备方法，其特征在于，以重量份数计，包括以下步骤：
S1：将44份650SN和10份150BS投入反应釜，搅拌升温至90℃，然后加水8份，加入2份氢氧化锂和0 .2份氢氧化钙，搅拌5min后，投入全部的3份癸二酸与7份12-羟基硬脂酸在125℃下皂化反应1 .5h；
S2：升温至140℃，脱水90分钟，继续升温至170℃，加入0.3份二苯胺，然后继续升温至215℃，高温炼制15分钟；
S3：加入21份650SN和5份150BS，并急速降温至160℃，在0 .8MPa下剪切2h；
S4：降温至90℃，加入2 .4份聚异丁烯、0 .5份辛基丁基二苯胺、2份磷酸胺、2份氨基硫代酯、0 .5份硫代磷酸三苯酯和0 .1份苯并三氮唑，搅拌均匀后，均质，过滤后即得复合锂基润滑脂。
2.通过如权利要求1中制备方法制得的复合锂基润滑脂。
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