CN115109629B - 一种高温润滑脂及其制备方法 - Google Patents

一种高温润滑脂及其制备方法 Download PDF

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CN115109629B
CN115109629B CN202210820444.4A CN202210820444A CN115109629B CN 115109629 B CN115109629 B CN 115109629B CN 202210820444 A CN202210820444 A CN 202210820444A CN 115109629 B CN115109629 B CN 115109629B
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贾展羽
高艳青
孙谦
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，具体涉及一种耐高温润滑脂组合物及其制备方法。所述耐高温润滑脂组合物按照重量份计，包括以下组分：稠化剂15～25份；基础油70～80份；极压抗磨剂0.5～3份；抗氧剂0.5～2份；所述基础油为酯类油和聚醚油；所述稠化剂为复合钛皂基稠化剂；所述极压抗磨剂选自二硫化钼、二烷基二硫代磷酸锌、碳酸钙、氧化硅、石墨和硅酸钙中的一种或多种。本发明的耐高温润滑脂具有大于300℃的滴点，良好的极压抗磨性和机械安定性，在高温下能够保持良好的润滑特性，避免流失，可向使用部位提供更可靠全面的防护，能够满足更高温度要求的复杂工况。

Description

一种高温润滑脂及其制备方法
技术领域
本发明涉及一种润滑脂技术领域，具体涉及一种高温润滑脂及其制备方法。
背景技术
润滑脂是一种将稠化剂分散在液体润滑剂内制备的固体至半流体产品，可以加入其他组分赋予其特殊性能。润滑脂同润滑油一样都是减少两个相对运动的表面之间的摩擦和磨损。
润滑脂在常温时是半固体状态，在高温或外力剪切作用下又可以像液体一样产生流动。相比润滑油等其他类型润滑剂，润滑脂除了能够提供润滑作用之外还具有防锈、密封、降震等功能。所以，在某些特定情况下必须使用润滑脂进行润滑，如：要求润滑剂必须具有密封作用防止外部灰尘、水分等杂质侵入；要求润滑剂必须附着在润滑部位等情况。
润滑脂在各行各业中都具有广泛的应用，包括冶金、交通运输、航天航空、家电、石油矿业、食品等，其中使用到润滑脂的零部件则主要包括轴承、链条、齿轮等。由于工业进程的不断发展，工业化水平的不断提高，对工业设备的要求越来越复杂，很多需要润滑的机械零部件使用的环境温度要求也越来越高，耐高温润滑脂的需求不断增加，高温润滑脂产品得到了快速发展契机，但是，目前市场上的高温润滑脂品种不够理想，大量高性能高温润滑脂依赖进口。所以，进行耐高温润滑脂品种的开发是非常有必要的。在润滑脂所有产品产量中，锂基润滑脂(包含复合锂基润滑脂)产量占比最大，而复合锂基润滑脂有良好的高温性，但是，随着新能源行业的发展锂资源紧缺，导致锂基润滑脂产品原料价格陡增，而钛金属在地壳中的含量丰盈，其在地壳中的丰度为0.6％，远高于锂的0.0065％，目前亟需提供一种复合钛基润滑脂品种。
发明内容
为了解决上述技术问题，本发明提供一种耐高温润滑脂及其制备方法。
第一方面，本发明提供的耐高温润滑脂组合物，按照重量份计，包括以下组分：
所述基础油为酯类油和聚醚油；所述稠化剂为复合钛皂基稠化剂；所述极压抗磨剂选自二硫化钼、二烷基二硫代磷酸锌、碳酸钙、氧化硅、石墨和硅酸钙中的一种或多种。本发明所提供的润滑脂采用科学设计的基础油，满足润滑脂耐高温的使用条件，稠化剂采用复合钛皂，结合优化添加的抗氧剂和极压抗磨剂，采用直接皂化法。其中配伍性能优良、价格适中的特定极压抗磨剂及抗氧剂，同时采用科学的组合，能够满足产品更高要求的耐高温性。本发明的耐高温复合钛润滑脂具有大于300℃的滴点，优异的极压抗磨性和机械安定性，在高温下能够保持良好的润滑特性，避免流失，可向使用部位提供更可靠全面的防护，能够满足更高温度要求的复杂工况。
作为优选，所述酯类油与聚醚油的质量比为3～5:1优选4:1。本发明中，采用上述混配方式的基础油，能够更好地提高润滑脂高温性能。
作为优选，所述稠化剂由小分子酸、中分子酸、高分子酸和有机钛为原料制得。
进一步优选，所述高分子酸为十二羟基硬脂酸、油酸的一种或两种，所述中分子酸为苯二甲酸、壬二酸、癸二酸的一种或多种，所述低分子酸为乙二酸、丙二酸、丁二酸、戊二酸中的一种或多种；优选的，所述高分子酸为十二羟基硬脂酸，所述中分子酸为苯二甲酸，所述低分子酸为乙二酸。
进一步优选，所述高分子酸与中分子酸质量比为6～8：3优选7:3，低分子酸与高、中分子酸加和质量比为1:5～1:9。
进一步优选，所述有机钛为四异丙醇钛酸酯。
本发明中，通过优选稠化剂中小分子酸、中分子酸、高分子酸和有机钛的种类，以及各种酸的比例调整使得该稠化剂在本发明体系中能够更好地发挥稠化作用，同时各种分子酸的相互作用能够进一步提高润滑脂的高温性能。
进一步优选，所述极压抗磨剂选自二硫化钼、二烷基二硫代磷酸锌、氧化硅、石墨和硅酸钙中的至少两种，优选为石墨、氧化硅和二硫化钼。
进一步优选，所述抗氧剂为胺类抗氧剂和/或酚类抗氧剂；优选的，所述酚类抗氧剂选自2,6-二叔丁基对甲苯酚、α-萘酚的一种或两种，所述酚类抗氧剂优选为2,6-二叔丁基对甲苯酚；和/或，所述胺类抗氧剂选自烷基化二苯胺、萘胺和对苯二胺中的一种或两种；所述胺类抗氧剂优选为烷基化二苯胺。
本发明中采用的极压抗磨剂尤其是优选种类，能够使得该润滑脂体系的极压抗磨性能得到进一步提高。同时其与抗氧剂共同作用有利于抗氧化性的提高。
进一步优选，按照重量份计，所述润滑脂组合物为以下重量份的组分：
第二方面，本发明提供的所述复合钛润滑脂组合物的制备方法，包括：将部分基础油，高分子酸、中分子酸和小分子酸混合，升温至60～80℃，然后加入有机钛，升温至90～150℃，皂化反应；加入部分基础油，加水升温至最高炼制温度190～220℃；加入剩余基础油，降温后加入抗氧剂和极压抗磨剂，进行后处理。本发明中，通过对制备工艺进行优化，尤其是在上述添加顺序和温度条件下，能够进一步提高润滑脂的性能，另外加水升温还能利于皂化，使反应更充分。
作为优选，本发明的耐高温润滑脂组合物的制备方法，包括：将30～50％基础油，高分子酸、中分子酸和小分子酸混合，升温至70～80℃，然后加入有机钛，升温至100～140℃，皂化反应90～150min；升温至最高炼制温度200～215℃，恒温3～5min；然后加入剩余基础油冷却降温，降温至80℃以下加入抗氧剂和极压抗磨剂，搅拌，进行分散、研磨，成品罐装。
本发明的有益效果至少在于：本发明提供的润滑脂，使用GB/T4929-85润滑脂滴点测定方法测试，滴点大于300℃，表示其可能使用的最高温度大于300℃，具有良好的耐高温性能。同时本发明所制备的润滑脂抗氧化性能很好，使用SH/T 0325方法测试，压力降可达18KPa。而且本发明所述的润滑脂，具有良好的极压性能，PD值可达到3632N。
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。
本发明以下实施例中，酯类油与聚醚油的质量比为4:1，所用酯类油具体为邻苯二甲酸二辛酯(DOP)，聚醚油为聚甲基硅醚。
实施例1
将稠化剂中42g十二羟基硬脂酸、18g苯二甲酸加入600g压釜油(即基础油)中，基础油为酯类油与聚醚油混配，升温至80℃，加入12g乙二酸，之后加入211g四异丙醇钛酸酯升温至130-140℃，进行皂化反应120min。反应完成后，加入805g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：2,6-二叔丁基对甲苯酚7.6g，烷基化二苯胺3.9g和极压抗磨剂：二硫化钼：9.4g；轻质碳酸钙18.9g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
实施例2
将稠化剂中56g十二羟基硬脂酸、24g苯二甲酸加入500g压釜油(即基础油)中，基础油为酯类油与聚醚油混配，升温至80℃，加入16g乙二酸，之后加入282.0g四异丙醇钛酸酯升温至130-140℃，进行皂化反应140min。反应完成后，加入810g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：2,6-二叔丁基对甲苯酚6.3g，烷基化二苯胺3.2g和极压抗磨剂：二硫化钼：11.3g；轻质碳酸钙7.6g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
实施例3
将稠化剂中49g十二羟基硬脂酸、21g苯二甲酸加入800g压釜油(即基础油)中，基础油为酯类油与聚醚油混配，升温至80℃，加入11.2g乙二酸，之后加入216.0g四异丙醇钛酸酯升温至130-140℃，进行皂化反应140min。反应完成后，加入638g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：2,6-二叔丁基对甲苯酚9g和极压抗磨剂：氧化硅11.2g；二硫化钼5.6g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
实施例4
将稠化剂中38.5g十二羟基硬脂酸、16.7g苯二甲酸加入500g压釜油(即基础油)中，基础油为酯类油与聚醚油混配，升温至80℃，加入7.7g乙二酸，之后加入170g四异丙醇钛酸酯升温至130-140℃，进行皂化反应140min。反应完成后，加入360g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：烷基化二苯胺15.6g和极压抗磨剂：石墨15.3g；氧化硅5.8g；二硫化钼7.3g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
实施例5
将稠化剂中59.5g十二羟基硬脂酸、25.5g苯二甲酸加入885g压釜油(即基础油)中，基础油为酯类油与聚醚油混配，升温至80℃，加入9.4g乙二酸，之后加入245.0g四异丙醇钛酸酯升温至130-140℃，进行皂化反应140min。反应完成后，加入700g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：2,6-二叔丁基对甲苯酚5.5g和极压抗磨剂：二烷基二硫代磷酸锌18.5g；二硫化钼13.5g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
对比例1
将稠化剂中50g十二羟基硬脂酸、12g苯二甲酸加入600g压釜油(即基础油)中，基础油为酯类油，升温至80℃，加入14g乙二酸，之后加入230.0g四异丙醇钛酸酯升温至130-140℃，进行皂化反应140min。反应完成后，加入600g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：2,6-二叔丁基对甲苯酚5g和极压抗磨剂：二烷基二硫代磷酸锌5g；二硫化钼2g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
对比例2
将稠化剂中35g十二羟基硬脂酸、22g苯二甲酸加入550g压釜油(即基础油)中，基础油为酯类油，升温至80℃，加入11g乙二酸，之后加入150.0g四异丙醇钛酸酯升温至130-140℃，进行皂化反应140min。反应完成后，加入400g基础油，之后，加水升温搅拌至200-215℃，加入剩余200g基础油冷却降温，降温至80℃加入全部抗氧剂：2,6-二叔丁基对甲苯酚8g和极压抗磨剂：二烷基二硫代磷酸锌12.5g，搅拌均匀后，经后处理设备分散研磨后成品罐装。
实验例1
对实施例1～5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1-5制备的润滑脂均表现出优异的耐高温性，良好的机械安定性能、极压抗磨性和氧化安定性。能够满足高温工况对润滑脂的更复杂的要求。
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 (5)

1.一种耐高温润滑脂组合物，其特征在于，按照重量份计，包括以下组分：
稠化剂 15~25份；
基础油 70~80份；
极压抗磨剂 0.5~3份；
抗氧剂 0.5~2份；
所述基础油为酯类油和聚醚油；所述酯类油与所述聚醚油的质量比为4:1，所述酯类油为邻苯二甲酸二辛酯，所述聚醚油为聚甲基硅醚；所述稠化剂为复合钛皂基稠化剂，所述稠化剂由小分子酸、中分子酸、高分子酸和有机钛为原料制得，所述高分子酸为十二羟基硬脂酸，所述中分子酸为苯二甲酸，所述低分子酸为乙二酸，所述高分子酸与中分子酸质量比为6~8：3，低分子酸与高、中分子酸加和质量比为1:5~1:9；所述极压抗磨剂为石墨、氧化硅和二硫化钼，所述抗氧剂为烷基化二苯胺。
2.根据权利要求1所述的耐高温润滑脂组合物，其特征在于，所述高分子酸与中分子酸质量比为7:3。
3.根据权利要求1或2所述的耐高温润滑脂组合物，其特征在于，所述有机钛为四异丙醇钛酸酯。
4.权利要求1~3任一项所述耐高温滑脂组合物的制备方法，其特征在于，包括：将部分基础油，高分子酸、中分子酸和小分子酸混合，升温至60~80℃，然后加入有机钛，升温至90~150℃，皂化反应；加入部分基础油，加水升温至最高炼制温度190~220℃；加入剩余基础油，降温后加入抗氧剂和极压抗磨剂，进行后处理。
5.根据权利要求4所述的耐高温润滑脂组合物的制备方法，其特征在于，将30~50%基础油，高分子酸、中分子酸和小分子酸混合，升温至70~80℃，然后加入有机钛，升温至100~140℃，皂化反应90~150min；升温至最高炼制温度200~215℃，恒温3~5min；然后加入剩余基础油冷却降温，降温至80℃以下加入抗氧剂和极压抗磨剂，搅拌，进行分散、研磨，成品罐装。
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