CN106753697A - 一种耐超高温复合多皂基自修复轴承润滑脂及其制备方法 - Google Patents

一种耐超高温复合多皂基自修复轴承润滑脂及其制备方法 Download PDF

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CN106753697A
CN106753697A CN201611055286.9A CN201611055286A CN106753697A CN 106753697 A CN106753697 A CN 106753697A CN 201611055286 A CN201611055286 A CN 201611055286A CN 106753697 A CN106753697 A CN 106753697A
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thickening agent
lubricating grease
additive
kettle
calcium
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CN106753697B (zh
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樊凤山
阎君
胡三德
廖顺知
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CHANGSHA ZHONGCHENG PETROCHEMICAL Co Ltd
Sinopec Oilfield Equipment Corp
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CHANGSHA ZHONGCHENG PETROCHEMICAL Co Ltd
Kingdream PLC
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Abstract

本发明涉及一种耐超高温复合多皂基自修复轴承润滑脂及其制备方法,该润滑脂由复合合成基础液、复合型稠化剂、高温抗氧添加剂、防腐蚀金属钝化剂、惰性极压添加剂、自修复添加剂、结构改进剂混合配制而成。本发明主要是在ZL200510120518.X和ZL 201210033794.2专利基础上对基础液、稠化剂、极压添加剂、耐磨添加剂等进行了优化,所得润滑脂不仅能够满足牙轮钻头轴承极压、高温、耐磨、自修复的润滑需求,还能在高达200℃以上温度环境下保持产品性能不变,避免造成钻头轴承失效,尤其适于在石油地质钻探领域中地热井、深地层的牙轮钻头轴承中使用,对于提高牙轮钻头轴承使用温度范围具有十分重要意义。

Description

一种耐超高温复合多皂基自修复轴承润滑脂及其制备方法
技术领域
本发明涉及一种耐超高温复合多皂基自修复轴承润滑脂及其制备方法,特别涉及用于石油地质勘探钻井地热、深井、高温领域牙轮钻头使用的复合多皂基自修复轴承润滑脂及其制备方法。
背景技术
随着页岩气、地热深井高温油气勘探的不断发展,行业内对勘探钻探工具的耐高温性能要求也相应不断提高,与之配套的勘探钻井所使用的牙轮钻头,其轴承的耐温性能的要求也更为苛刻。
石油地质勘探钻井使用的油用牙轮钻头,在勘探过程中钻头轴承面临着极高的摩擦生热,钻头轴承的超高压、高冲击负荷,接触面因摩擦产生的高温对钻头轴承润滑脂提出了更高的耐温性要求。钻井高温也会造成润滑脂内部的化学物质之间发生反应,这种润滑脂内部的反应往往会造成润滑脂性能的变化,最终可能导致钻头轴承过早失效,从而危及牙轮钻头使用寿命。
在目前公开的文献资料中,针对环境温度对牙轮钻头轴承润滑脂性能的影响已有相当多的介绍。如美国休斯公司在其钻头轴承测试试验中发现,高温会造成钻头轴承过早失效;斯密斯公司也进行过相似的测试试验,试验结果表明:钻头轴承润滑脂在温度达到150℃后,其本身的极压抗磨性能会急剧下降。
本发明是专利ZL 200510120518.X和ZL 201210033794.2的继续与延伸,主要目的是大幅度提高润滑脂的耐温性能。本申请人针对专利ZL200510120518.X和ZL201210033794.2研制的轴承润滑脂进行了相似的高温极压性能测试。参照润滑脂极压耐磨性能评价方法——润滑脂极压性能测定法,SH/T 0202(四球法)和SH/T 0203(梯姆肯试验机法),ZL 200510120518.X和ZL 201210033794.2的两款专利产品在150℃高温条件下的烧结负荷均为400KG、Timken试验仅为40 1bf,而重载耐磨试验620kg-900rpm-300s无法完成,证明150℃的高温对润滑脂的性能造成了明显影响,使产品的极压抗磨性能明显下降。如何在保证牙轮钻头轴承润滑脂本身性能不下降的同时让牙轮钻头轴承润滑脂拥有更高的耐温性能就成为目前润滑材料领域的技术难题。
本发明充分考虑到专利ZL 200510120518.X和ZL 201210033794.2中采用的基础液、稠化剂和添加剂本身的耐高温性能,同时充分考虑到不同组分或原料间的相互反应作用,在此基础上,本申请对原专利中的基础液、稠化剂、添加剂配方均进行了优化,通过采用高温稳定性更好的原材料并考虑原材料间相互配伍作用,使本申请所提供的润滑脂在基本性能不下降的前提下,较大幅度提升润滑脂的耐高温性能。
发明内容
本发明所要解决的技术问题是针对专利ZL 200510120518.X和ZL201210033794.2产品中耐高温性能不足,提供一种耐超高温复合多皂基自修复轴承润滑脂及其制备方法,该润滑脂不仅能够满足牙轮钻头轴承极压、高温、耐磨、自修复的润滑需求,还能在高达200℃温度的环境下保持产品性能不变,避免因润滑脂在高温条件下性能下降而造成钻头轴承失效。
为解决上述技术问题,本发明提供的技术方案是:
提供一种耐超高温复合多皂基自修复轴承润滑脂,其包含复合合成基础液、复合型稠化剂、高温抗氧添加剂、防腐蚀金属钝化剂、惰性极压抗磨添加剂、自修复添加剂、结构改进剂混合配制而成,各组分含量按重量计为:
按上述方案,所述的复合合成基础液按重量计由合成聚合物聚α-烯烃PAO1501~25份,合成聚合物聚α-烯烃PAO20 1~25份,烷基萘1~25份,合成多元醇酯5~50份,合成偏苯酯5~50份,全氟聚醚0~25份组成。
按上述方案,所述的复合型稠化剂按重量计由复合钙基稠化剂1~25份、有机膨润土稠化剂1~25份组成。
按上述方案,所述复合钙基稠化剂由氢氧化钙与C8酸、12-羟基硬脂酸、C2酸钙盐发生反应复合制得,其组分含量按重量计包含氢氧化钙1~5份、C2酸钙盐1~25份、C8酸0~25份、12-羟基硬脂酸1~25份;所述C2酸钙盐为微米级,平均粒径5~15um,有效含量99%;
所述有机膨润土稠化剂由有机膨润土与水、酒精、丙酮中的一种或多种发生反应制得,其组分含量按重量计包含有机膨润土1~25份、水0~5份、酒精0~5份、丙酮0~5份,水、酒精和丙酮的总量不低于0.5份、不高于10份。
按上述方案,所述高温抗氧添加剂选取酚型、胺型或酚胺型抗氧添加剂中的一种或多种;所述防腐蚀金属钝化剂选取苯三唑衍生物、噻二唑衍生物或杂环化合物添加剂中的一种或多种。
按上述方案,所述惰性极压添加剂按重量计包含二硫化钨5~25份、极化石墨5~25份、氮化硼5~25份、纳米碳酸钙5~25份;
所述惰性极压添加剂为微米级,325目筛网通过率90%,有效含量99%,其中所述极化石墨为微米级,平均粒径5~15um,有效含量99%;所述氮化硼为微米级,平均粒径10~30um,有效含量99%;所述纳米碳酸钙平均粒径20~30nm,有效含量60~70%。
按上述方案,所述自修复添加剂按重量计包含纳米级银、铜、锌金属粉末类物质填充剂的一种或几种1~10份,氧化镁0~5份,二氧化钛0~5份,铋、锆的氧化物或铋、锆乙烯基化合物0~10份。
按上述方案,所述结构改进剂为丙三醇。
本发明还提供上述耐超高温复合多皂基自修复轴承润滑脂的制备方法,其特征在于第一步分别在炼制釜和调和釜内调制部分基础液作为反应介质,第二步在调和釜内在反应介质基础液中进行有机膨润土稠化剂的制备,第三步在炼制釜内在反应介质基础液中进行复合钙基稠化剂的制备,第四步在调和釜内进行有机膨润土稠化剂和复合钙基稠化剂的复合,第五步在调和釜内进行各添加剂添加和均化、剪切、调和、脱气、包装。
按上述方案,所述反应介质基础液的调制过程为:在炼制釜内按比例依次加入PAO150、PAO20、烷基萘、全氟聚醚,升温、调制成均匀介质,待用;在调和釜内按照比例依次加入合成多元醇酯、合成偏苯酯,升温、调制成均匀介质,待用;
所述有机膨润土稠化剂制备过程为:在调和釜内在反应介质复合合成基础液中加入有机膨润土,充分搅拌,时间不低于30min,加热升温至大约50摄氏度,加入水、酒精、丙酮中的一种或多种,反应30min后,升温至大约100摄氏度,循环搅拌,脱除酒精和丙酮,时间不低于60min,制备完成后待用;
所述复合钙基稠化剂制备过程为:在炼制釜内在反应介质复合合成基础液中加入氢氧化钙,充分搅拌,时间不低于40min,加热升温至大约60摄氏度,加入C8酸,时间不低于20min,然后加入12-羟基硬脂酸,时间不低于20min,反应20min后加入C2酸钙盐复合炼制,然后升温至100℃反应脱水,然后升温至120℃,取样测定基础皂样游离酸碱含量,用12-羟基硬脂酸调节控制游离碱的含量为0.01~0.05NAOH%,然后稠化,升温至160℃时加入丙三醇,继续升温至最高炼制温度200~220℃,恒温20min;
所述复合型稠化剂制备过程为:将炼制釜内制备完成的复合钙基稠化剂用泵转至调和釜,与调和釜内的有机膨润土稠化剂在120~160℃温度下反应45min,然后冷却至100℃以下;
所述添加剂添加和均化、剪切、调和、脱气、包装过程:在调和釜内对降温后的基础脂进行搅拌、循环、保温,依次加入二硫化钨粉体、极化石墨、氮化硼、纳米碳酸钙,搅拌循环60min后加入高温抗氧添加剂、防腐蚀金属钝化剂,然后加入自修复添加剂并充分循环搅拌,最后均质、剪切、脱气至成品。
本申请为提高润滑脂的耐高温性能,对原专利中的基础液、稠化剂、添加剂配方均进行了优化,在维持牙轮钻头轴承润滑脂优异的极压、耐磨性能的同时,大幅度提高润滑脂的耐高温性能。本专利所属产品在综合性能上更加优异,耐高温性能更加突出,极压性能维持较高水平。
本发明具有的技术特点:一是在ZL 201210033794.2专利基础上,通过对原专利中的基础液、稠化剂、添加剂配方进行优化,在维持牙轮钻头轴承润滑脂优异的极压、耐磨性能的前提下,提高润滑脂的耐高温性能;二是采用的复合合成基础液,由几种高温性能优良同时性能各有补充的合成基础油组成一种复合合成基础液,其中新引入了合成多元醇酯和合成偏苯酯基础油原料,使润滑脂产品的高温稳定性和高温润滑性得到明显改善;三是采用的复合型稠化剂,与ZL 201210033794.2专利一样,将复合钙基稠化剂作为基本稠化剂,更为不同的是,为了加强稠化剂本身的耐高温性能,本专利所属复合型稠化剂引入了部分有机膨润土稠化剂与复合钙基稠化剂复合成复合型稠化剂,由于膨润土稠化剂的高温稳定性极佳,在高温环境下其本身皂纤维结构十分稳定,且可将其他组分物质分散在其皂纤维结构中防止高温下发生反应,因此,对提高润滑脂性能的高温稳定性起到积极作用;四是采用的惰性极压抗磨添加剂与ZL 201210033794.2专利一样仍然采用了二硫化钨、极化石墨等,更为不同的是,为提高润滑脂高温极压抗磨性能,采用了氮化硼、纳米碳酸钙作为极压抗磨添加剂,并对不同的极压抗磨添加剂进行了合理配比。
本发明的有益效果在于:
1.本发明采用了高温稳定性更好的复合合成基础液、复合型稠化剂、惰性极压抗磨添加剂等原材料,使润滑脂具有优异的极压、耐磨性能的同时提高润滑脂耐温性能。随着我国未来油气勘探的发展,对勘探技术的要求也相应提高。针对地热井、深地层油气勘探,普通牙轮钻头轴承润滑脂产品在高温环境下,其产品性能会急剧下降,最终可能导致钻头轴承过早失效,从而危及牙轮钻头使用寿命。因此,提高牙轮钻头轴承润滑脂自身的耐高温性能,是保证牙轮钻头轴承在高温环境下正常运转的必要条件。本发明通过提高原材料自身的耐高温性能,如本专利采用的复合合成基础油高温蒸发损失更低、复合型稠化剂的高温稳定性更好、惰性极压抗磨添加剂的高温极压抗磨性能更好。同时对不同原料之间的协同作用进行了合理配伍,如采用的复合合成基础液能同时适合复合钙基润滑脂和膨润土基润滑脂;而惰性极压抗磨添加剂的搭配也使其对产品极压抗磨性能的改善效果达到最佳,高温和常温条件下的烧结负荷均能达到800kg。因此本发明专利润滑脂产品在维持牙轮钻头轴承润滑脂优异的性能和满足环保要求的前提下,提高润滑脂的耐高温性能。
2.本发明采用多种高温性能优良的合成基础油调配成复合合成基础液,利用不同类别合成基础油的特性,按不同比例进行调和,使最终的复合合成基础液具有极高的粘度指数,极高的闪点,优异的高低温稳定性能同时,能更好的与稠化剂、添加剂进行协调作用。其中新引入的合成多元醇酯和合成偏苯酯基础油原料,使润滑脂产品的高温稳定性和高温润滑性得到明显改善。
3.本发明采用复合型稠化剂,一种以复合钙基稠化剂与有机膨润土稠化剂复合的复合型稠化剂,该复合型稠化剂在保持复合钙皂极压高承载、抗水的特性外,通过有机膨润土稠化剂的引入,有效的提高了润滑脂高温结构稳定性,从而提高润滑脂的耐高温性能。
4.本发明采用多种惰性极压抗磨添加剂配伍使用。其采用的惰性极压添加剂为微米级,325目筛网通过率90%,有效含量99%;采用的极化石墨耐磨添加剂为微米级,平均粒径5~15um,有效含量99%;采用的氮化硼为微米级,平均粒径10~30um,有效含量99%。采用的碳酸钙为纳米级,平均粒径20~30nm,有效含量60~70%。;
5.本发明采用的胺型、酚型或酚胺型抗氧抗腐蚀添加剂与苯三唑衍生物、噻二唑衍生物或杂环化合物添加剂组成金属钝化剂有很好的协同效应,能有效克服现代钻头轴承技术中采用的有色金属合金如焊铜合金而面临的抗腐蚀问题。
6.本发明采用自修复复合型添加剂,按重量计包含纳米金属粉末类物质如银、铜、锌填充剂0~8份,还包含羟基硅酸镁聚合物0~5份或氟碳聚合物或聚四氟乙烯0~5份,还包括铋、锆的氧化物或乙烯基化合物0~10份。以上极压添加剂、耐磨添加剂、自修复添加剂协同作用后形成的复合型极压耐磨添加剂能够完成使润滑脂摩擦磨损性能达到极其优异程度,按照润滑脂极压耐磨性能评价四球烧结负荷高于800KG,Timken试验超过100 1bf,重载耐磨试验620kg‐900rpm‐300s低于1.45mm。
7.本发明润滑脂在维持牙轮钻头轴承润滑脂优异的极压、耐磨性能的前提下,有效提高润滑脂的耐高温性能。产品工作锥入度不高于340mm 1/10,6万次工作锥入度不高于370mm1/10,滴点不低于330℃,极压烧结负荷高于800kg,综合磨损指数大于160,抗擦伤能力大于100 1bf,200℃条件下的极压烧结负荷不低于800,200℃的高温蒸发损失不高于5%。
总之,本发明是ZL 200510120518.X专利和ZL 201210033794.2专利延伸与发展,主要是采用了高温稳定性更好的原材料,如复合合成基础液、氮化硼和轻质碳酸钙等惰性极压添加剂等,使润滑脂具有优异的耐高温温性能,从而有效满足钻头轴承的耐高温适用范围,尤其适于在石油地质钻探领域中地热井、深地层的牙轮钻头轴承中使用,对于提高牙轮钻头轴承使用温度范围具有十分重要意义。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案,下面结合实施例对本发明作进一步详细描述。
实施例1
由以下组分和含量的原料按重量计配制而成:
制备方法:
在调和釜按照计量分别加入12份合成多元醇酯,搅拌状态下均匀加入6份合成偏苯酯调和均匀后,加入9份有机膨润土,充分搅拌,时间不低于30min,然后加热调和釜至50℃,加入2份酒精,反应30min后,继续升温至100℃,搅拌分散,脱除酒精,时间不低于60min,制备完毕,待用;
在炼制釜内按照计量分别加入12份PAO150,搅拌状态下均匀依次加入6份PAO20、4份烷基萘、2份合成氟化聚醚调和均匀,加热搅拌炼制釜至60℃,加入3份氢氧化钙粉体,充分搅拌,时间不低于40min,然后加入1.5份辛酸,时间不低于20min,然后加入3份12-羟基硬脂酸,时间不低于20min,反应20min后,加入6份醋酸钙粉体,时间不低于30min,然后升温反应,至100℃,反应脱水,至120℃,测溶液中基础皂样测定游离酸碱量,用适量的12-羟基硬脂酸调节游离碱的含量为0.01~0.05NAOH%,然后继续升温至160℃时加入1份丙三醇,继续升温至最高炼制温度200~220℃,恒温20min。
用泵将炼制釜中的物料转至调和釜,在120~160℃温度下,反应45min,然后搅拌循环冷却至100℃以下;
依次加入6份二硫化钨粉体、6份极化石墨粉体、10份氮化硼粉体、6份纳米碳酸钙粉体,搅拌循环120min后加入二苯胺抗氧化添加剂0.5份、烷基噻二唑金属钝化剂0.5份,循环搅拌45min,然后加入0.5份氧化镁、0.5份氧化钛、2份纳米金属银膏体、1.5份氧化铋粉体,循环均质、剪切、脱气、至成品包装。
通过上述程序生产的润滑脂其60次工作锥入度为322mm 1/10,滴点356℃,Cu T3100℃1A级,烧结负荷大于800KG,OK值105 1bf,综合磨损值171,200℃条件下的极压烧结负荷800KG,200℃的高温蒸发损失3.5%。
实施例2
由以下组分和含量的原料按重量计配制而成:
制备方法:
在调和釜按照计量分别加入6份合成多元醇酯,搅拌状态下均匀加入12份合成偏苯酯调和均匀后,加入6份有机膨润土,充分搅拌,时间不低于30min,然后加热调和釜至50℃,加入1.5份酒精,反应30min后,继续升温至100℃,搅拌分散,脱除酒精,时间不低于60min,制备完毕,待用;
在炼制釜内按照计量分别加入15份PAO150,搅拌状态下均匀依次加入3份PAO20、3份烷基萘、3份合成氟化聚醚调和均匀,加热搅拌炼制釜至60℃,加入4份氢氧化钙粉体,充分搅拌,时间不低于40min,然后加入1.5份辛酸,时间不低于20min,然后加入4份12-羟基硬脂酸,时间不低于20min,反应20min后,加入7.5份醋酸钙粉体,时间不低于30min,然后升温反应,至100℃,反应脱水,至120℃,测溶液中基础皂样测定游离酸碱量,用适量的12-羟基硬脂酸调节游离碱的含量为0.01~0.05NAOH%,然后继续升温至160℃时加入1份丙三醇,继续升温至最高炼制温度200~220℃,恒温20min。
用泵将炼制釜中的物料转至调和釜,在120~160℃温度下,反应45min,然后搅拌循环冷却至100℃以下;
依次加入4份二硫化钨粉体、8份极化石墨粉体、12份氮化硼粉体、4份纳米碳酸钙粉体,搅拌循环120min后加入二苯胺抗氧化添加剂0.5份、烷基噻二唑金属钝化剂0.5份,循环搅拌45min,然后加入1份氧化镁、0.5份氧化钛、2份纳米金属银膏体、1份氧化铋粉体,循环均质、剪切、脱气、至成品包装。
通过上述程序生产的润滑脂其60次工作锥入度为316mm 1/10,滴点360℃,Cu T3100℃1A级,烧结负荷大于800KG,OK值105 1bf,综合磨损值176,200℃条件下的极压烧结负荷800KG,200℃的高温蒸发损失3.2%。
实施例3
由以下组分和含量的原料按重量计配制而成:
制备方法:
在调和釜按照计量分别加入9份合成多元醇酯,搅拌状态下均匀加入9份合成偏苯酯调和均匀后,加入11份有机膨润土,充分搅拌,时间不低于30min,然后加热调和釜至50℃,加入2.5份酒精,反应30min后,继续升温至100℃,搅拌分散,脱除酒精,时间不低于60min,制备完毕,待用;
在炼制釜内按照计量分别加入9份PAO150,搅拌状态下均匀依次加入9份PAO20、3份烷基萘、3份合成氟化聚醚调和均匀,加热搅拌炼制釜至60℃,加入2.5份氢氧化钙粉体,充分搅拌,时间不低于40min,然后加入1份辛酸,时间不低于20min,然后加入2.5份12-羟基硬脂酸,时间不低于20min,反应20min后,加入5份醋酸钙粉体,时间不低于30min,然后升温反应,至100℃,反应脱水,至120℃,测溶液中基础皂样测定游离酸碱量,用适量的12-羟基硬脂酸调节游离碱的含量为0.01~0.05NAOH%,然后继续升温至160℃时加入1份丙三醇,继续升温至最高炼制温度200~220℃,恒温20min。
用泵将炼制釜中的物料转至调和釜,在120~160℃温度下,反应45min,然后搅拌循环冷却至100℃以下;
依次加入8份二硫化钨粉体、4份极化石墨粉体、8份氮化硼粉体、8份纳米碳酸钙粉体,搅拌循环120min后加入二苯胺抗氧化添加剂0.5份、烷基噻二唑金属钝化剂0.5份,循环搅拌45min,然后加入0.5份氧化镁、1份氧化钛、2份纳米金属银膏体、1份氧化铋粉体,循环均质、剪切、脱气、至成品包装。
通过上述程序生产的润滑脂其60次工作锥入度为337mm 1/10,滴点354℃,Cu T3100℃1A级,烧结负荷大于800KG,OK值105 1bf,综合磨损值168,200℃条件下的极压烧结负荷800KG,200℃的高温蒸发损失3.7%。

Claims (10)

1.一种耐超高温复合多皂基自修复轴承润滑脂,其特征在于包含复合合成基础液、复合型稠化剂、高温抗氧添加剂、防腐蚀金属钝化剂、惰性极压抗磨添加剂、自修复添加剂、结构改进剂混合配制而成,各组分含量按重量计为:
2.按权利要求1所述的耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述的复合合成基础液按重量计由合成聚合物聚α-烯烃PAO150 1~25份,合成聚合物聚α-烯烃PAO20 1~25份,烷基萘1~25份,合成多元醇酯5~50份,合成偏苯酯5~50份,全氟聚醚0~25份组成。
3.按权利要求1或2所述耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述的复合型稠化剂按重量计由复合钙基稠化剂1~25份、有机膨润土稠化剂1~25份组成。
4.按权利要求3所述的耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述复合钙基稠化剂由氢氧化钙与C8酸、12-羟基硬脂酸、C2酸钙盐发生反应复合制得,其组分含量按重量计包含氢氧化钙1~5份、C2酸钙盐1~25份、C8酸0~25份、12-羟基硬脂酸1~25份;所述C2酸钙盐为微米级,平均粒径5~15um,有效含量99%;
所述有机膨润土稠化剂由有机膨润土与水、酒精、丙酮中的一种或多种发生反应制得,其组分含量按重量计包含有机膨润土1~25份、水0~5份、酒精0~5份、丙酮0~5份,水、酒精和丙酮的总量不低于0.5份、不高于10份。
5.按权利要求1或2所述的耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述高温抗氧添加剂选取酚型、胺型或酚胺型抗氧添加剂中的一种或多种;所述防腐蚀金属钝化剂选取苯三唑衍生物、噻二唑衍生物或杂环化合物添加剂中的一种或多种。
6.按权利要求1或2所述的耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述惰性极压添加剂按重量计包含二硫化钨5~25份、极化石墨5~25份、氮化硼5~25份、纳米碳酸钙5~25份;
所述惰性极压添加剂为微米级,325目筛网通过率90%,有效含量99%,其中所述极化石墨为微米级,平均粒径5~15um,有效含量99%;所述氮化硼为微米级,平均粒径10~30um,有效含量99%;所述纳米碳酸钙平均粒径20~30nm,有效含量60~70%。
7.按权利要求1或2所述的耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述自修复添加剂按重量计包含纳米级银、铜、锌金属粉末类物质填充剂的一种或几种1~10份,氧化镁0~5份,二氧化钛0~5份,铋、锆的氧化物或铋、锆乙烯基化合物0~10份。
8.按权利要求1或2所述的耐超高温复合多皂基自修复轴承润滑脂,其特征在于所述结构改进剂为丙三醇。
9.一种按权利要求1-8任一所述的耐超高温复合多皂基自修复轴承润滑脂的制备方法,其特征在于第一步分别在炼制釜和调和釜内调制部分基础液作为反应介质,第二步在调和釜内在反应介质基础液中进行有机膨润土稠化剂的制备,第三步在炼制釜内在反应介质基础液中进行复合钙基稠化剂的制备,第四步在调和釜内进行有机膨润土稠化剂和复合钙基稠化剂的复合,第五步在调和釜内进行各添加剂添加和均化、剪切、调和、脱气、包装。
10.按权利要求9所述的耐超高温复合多皂基自修复轴承润滑脂的制备方法,其特征在于:
所述反应介质基础液的调制过程为:在炼制釜内按比例依次加入PAO150、PAO20、烷基萘、全氟聚醚,升温、调制成均匀介质,待用;在调和釜内按照比例依次加入合成多元醇酯、合成偏苯酯,升温、调制成均匀介质,待用;
所述有机膨润土稠化剂制备过程为:在调和釜内在反应介质复合合成基础液中加入有机膨润土,充分搅拌,时间不低于30min,加热升温至大约50摄氏度,加入水、酒精、丙酮中的一种或多种,反应30min后,升温至大约100摄氏度,循环搅拌,脱除酒精和丙酮,时间不低于60min,制备完成后待用;
所述复合钙基稠化剂制备过程为:在炼制釜内在反应介质复合合成基础液中加入氢氧化钙,充分搅拌,时间不低于40min,加热升温至大约60摄氏度,加入C8酸,时间不低于20min,然后加入12-羟基硬脂酸,时间不低于20min,反应20min后加入C2酸钙盐复合炼制,然后升温至100℃反应脱水,然后升温至120℃,取样测定基础皂样游离酸碱含量,用12-羟基硬脂酸调节控制游离碱的含量为0.01~0.05NAOH%,然后稠化,升温至160℃时加入丙三醇,继续升温至最高炼制温度200~220℃,恒温20min;
所述复合型稠化剂制备过程为:将炼制釜内制备完成的复合钙基稠化剂用泵转至调和釜,与调和釜内的有机膨润土稠化剂在120~160℃温度下反应45min,然后冷却至100℃以下;
所述添加剂添加和均化、剪切、调和、脱气、包装过程:在调和釜内对降温后的基础脂进行搅拌、循环、保温,依次加入二硫化钨粉体、极化石墨、氮化硼、纳米碳酸钙,搅拌循环60min后加入高温抗氧添加剂、防腐蚀金属钝化剂,然后加入自修复添加剂并充分循环搅拌,最后均质、剪切、脱气至成品。
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