CN107384558B - 以插层型层状磷酸镁作为固体润滑添加剂的润滑脂及其制备方法 - Google Patents

以插层型层状磷酸镁作为固体润滑添加剂的润滑脂及其制备方法 Download PDF

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CN107384558B
CN107384558B CN201710645563.XA CN201710645563A CN107384558B CN 107384558 B CN107384558 B CN 107384558B CN 201710645563 A CN201710645563 A CN 201710645563A CN 107384558 B CN107384558 B CN 107384558B
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grease
magnesium
lubricating grease
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董晋湘
张效胜
徐红
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Taiyuan University of Technology
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Abstract

本发明公开了一种以插层型层状磷酸镁作为固体润滑添加剂的润滑脂及其制备方法。该润滑脂由以下重量份数的组分组成:基础润滑脂79‑98.95份,插层型层状磷酸镁材料1.0‑10.0份,抗氧剂0.05‑5.0份,防锈剂0‑6.0份;所述的基础润滑脂包括基础锂基润滑脂或基础复合锂基润滑脂。制备方法为:将基础润滑脂、插层型层状磷酸镁材料、抗氧剂和防锈剂在室温‑200℃下搅拌混合1‑10 h,利用三辊机或高压均质机研磨均化0.5‑3h使之均匀,制得润滑脂产品。本发明提供的含有插层型层状磷酸镁材料作为固体润滑添加剂的润滑脂具有良好的承载抗磨减摩能力,易于实现工业化。

Description

以插层型层状磷酸镁作为固体润滑添加剂的润滑脂及其制备 方法
技术领域
本发明属于一种润滑脂及制备方法,具体涉及以插层型层状磷酸镁材料作为固体润滑添加剂的润滑脂及其制备方法。
背景技术
工业生产中,80 %的机械失效是磨损失效,影响设备效率的各种因素中,1 / 3 -1 / 2的的能耗是由摩擦副摩擦磨损引起的。我国每年各类机械因润滑不良造成的损失超过国民生产总值的3 %。润滑脂和脂润滑是一种有效的工业润滑选择,越来越受到人们的重视。目前全球润滑脂产量稳定在75万吨左右,其中锂基润滑脂和复合锂基润滑脂占全年润滑脂总产量的70 %,是最重要的润滑脂品种。随着工业技术的发展,机械运转工况日益复杂,对润滑脂的各种性能要求也日益苛刻,要求润滑脂可以在更高温度、更高载荷、更高DN值等工况长期有效工作。通常需要在润滑脂里面添加固体润滑添加剂,其最重要的作用是当基础润滑脂的润滑膜在遭受重负荷、振动、冲击负荷或高温的情况下起补强的作用,可有效改善脂的润滑性、抗磨性和抗擦伤性。目前为止,常用的固体润滑添加剂为二硫化钼、石墨,公认的原因是它们具有层状晶体结构,与基础平面平行的层间结合力弱,故晶体中间易于平行滑动,即内摩擦力小。但这两种材料还存在着缺陷,如材料成本高、色泽重、应用工况范围限制等,需要开发新型有效固体润滑添加剂。
固体润滑添加剂材料的选择需要考虑经济成本,资源丰富,价格低廉的材料值得重视。镁是地壳中分布最广泛的元素之一,占第八位,质量百分含量达到2.0 %。层状磷酸镁材料是一类主体层板由MgO6八面体、PO4四面体构成的无机化合物,在微观尺度上具有与传统固体润滑添加剂二硫化钼、石墨类似的层状晶体结构。本课题组前期在专利CN103264999中报道了离子液体热合成一种镁离子交换型层状磷酸镁(Mg4P4H14O21)作为润滑油添加剂,可以有效改善润滑性能。氮、磷是典型的润滑抗磨元素,在层状磷酸镁材料层间可以引入无机铵和有机胺分子,形成一系列插层型层状磷酸镁材料,有望表现出更加优异的抗磨减摩能力,目前尚未有插层型层状磷酸镁材料作为润滑脂固体润滑添加剂的报道。
发明内容
本发明的内容是提供一种具有良好承载抗磨减摩性能的含有插层型层状磷酸镁材料作为固体润滑添加剂的锂基润滑脂和复合锂基润滑脂及其制备方法。
本发明润滑脂的质量份数组成为:
基础润滑脂79 - 98.95份,插层型层状磷酸镁材料1.0 - 10.0份,抗氧剂0.05 -5.0份,防锈剂0 - 6.0份。优选组成范围为基础润滑脂85 - 95份,插层型层状磷酸镁材料3.0 - 7.0份,抗氧剂0.05 - 3.0份,防锈剂0 - 4.0份。
如上所述的基础润滑脂包括基础锂基润滑脂、基础复合锂基润滑脂。
如上所述的基础锂基润滑脂可以由包括脂肪酸,基础油和氢氧化锂在内的原料反应、混合而成,其中脂肪酸5.0 - 30.0份,基础油70.0 - 95.0份,氢氧化锂0.2 - 3.0份;基础锂基润滑脂的制备方法:将1 / 3 基础油倒入制脂釜中,启动搅拌器,加热升温至70 -80 ℃,投入脂肪酸,待脂肪酸完全溶解,再加入预先溶于水的氢氧化锂溶液,温度控制在120 - 130 ℃之间,反应1 - 5 h。皂化结束后加入1 / 3基础油,温度控制在200 - 220 ℃之间,持续10 min 后,停止加热。温度降到160 - 190 ℃时,加入1 / 3 基础油,体系降温至100 ℃时,停止搅拌,用三辊机或高压均质机研磨均匀后即得基础锂基润滑脂。
如上所述的基础复合锂基润滑脂可以由包括脂肪酸、复合剂、氢氧化锂和基础油在内的原料反应、混合而成,其中脂肪酸4.0 - 10.0份,复合剂1.0 - 5.0份,氢氧化锂1.0- 4.0份,基础油81.0 - 94.0份;基础复合锂基润滑脂的制备方法:向制脂釜中加入1 / 3基础油,脂肪酸,升温熔化,慢慢加入1 / 2 的氢氧化锂水溶液,温度为80 - 115 ℃。加完氢氧化锂溶液后,温度迅速升至130 - 180 ℃,使皂基脱水完全,物料快冷至90 - 115 ℃,加入复合剂,搅拌10 min,慢慢加入1/2 氢氧化锂水溶液,使复合剂皂化,温度升至130 -180 ℃保持1 h 使脱水完全,迅速升温至200 - 220 ℃并保持20 min,加入2 / 3 基础油,使脂基迅速冷却,继续搅拌冷却至66 ℃,用三辊机或高压均质机研磨均匀后即得基础复合锂基润滑脂。
所述的脂肪酸包括12-羟基硬脂酸或硬脂酸。
所述的基础油选自烃类基础油、酯类基础油和硅油类基础油中的一种或几种,任意比混合。
所述的烃类基础油是指石蜡基矿物油、环烷基矿物油、中间基矿物油、合成烃中的一种;
所述酯类基础油是指双酯油、多元醇酯油、复酯油、偏苯三酸酯油中的一种;
所述硅油类基础油是指甲基硅油、乙基硅油、甲苯基硅油、二苯基硅油中的一种;
所述的复合剂为己二酸、辛二酸、癸二酸中的一种;
所述的插层型层状磷酸镁材料为无机铵根和有机胺(乙二胺、1,3-丙二胺、1,4-丁二胺、1,6-己二胺)插层型层镁MgNH4PO4·H2O、0.5·[NH3(CH2)2NH3]2+·[MgPO4·H2O]-(MgP-EDA)、0.5·[NH3(CH2)3NH3]2+·[MgPO4·H2O]- (MgP-PDA)、0.5·[NH3(CH2)4NH3]2+·[MgPO4·H2O]- (MgP-DAB)和0.5·[NH3(CH2)6NH3]2+·[MgPO4·H2O]- (MgP-HMD)。
所述无机铵根插层型层镁的制备方法是将原料镁源、磷酸、无机铵盐在水溶液中反应,反应温度为25 - 300 ℃,反应时间0.1 - 8天,经过滤、蒸馏水洗涤,室温干燥后获得;原料配比为磷镁摩尔比(1-10):1,铵镁摩尔比(1-10):1和水镁摩尔比(5-100):1;
所述无机铵盐为氯化铵、尿素、氨水中的一种;镁源为氯化镁、醋酸镁、无定型磷酸镁中的一种。
所述有机胺插层型层镁的制备方法是将原料镁源、磷酸、有机胺在水溶液中反应,反应温度为25 - 250 ℃,反应0.1 - 8天,经过滤、蒸馏水洗涤,室温干燥后获得;原料配比为磷镁摩尔比(1-10):1,胺镁摩尔比(1-10):1和水镁摩尔比(5-100):1;
有机胺为乙二胺、1,3-丙二胺、1,4-丁二胺、1,6-己二胺中的一种;镁源为氯化镁、醋酸镁、无定型磷酸镁中的一种。
所述的抗氧剂包括2, 6-二叔丁基对甲苯酚、β-萘酚、二苯胺、吩噻嗪中的一种。
所述的防锈剂包括烯基丁二酸、十二烯基丁二胺、苯并三氮唑中的一种。
本发明润滑脂的制备方法包括如下步骤:将基础润滑脂、插层型层状磷酸镁材料、抗氧剂和防锈剂在室温 - 200 ℃下搅拌混合1 - 10 h,利用三辊机或高压均质机研磨均化0.5 - 3 h使之均匀,制得润滑脂产品。
本发明的优点和有益效果如下:
(1) 本发明首次报道含有插层型层状磷酸镁材料作为固体润滑添加剂的锂基和复合锂基润滑脂的制备,开发出新型系列润滑脂。
(2) 本发明报道含有插层型层状磷酸镁材料作为固体润滑添加剂的锂基和复合锂基润滑脂中所含有的层状磷酸镁原料来源丰富,价格低廉,可有效降低工业应用的成本。
(3) 本发明报道含有插层型层状磷酸镁材料作为固体润滑添加剂的锂基和复合锂基润滑脂具有良好的承载抗磨减摩能力,制备方法简便易行,易于实现工业化。
具体实施方式
下面是本发明的具体的实施方式,实施例仅是说明性的,不能以此来限制本发明的保护范围。
实施例 1
将31.7 g PAO8倒入制脂釜中,启动搅拌器,加热升温至70 ℃,投入5.0 g 12-羟基硬脂酸,待12-羟基硬脂酸完全溶解,再加入预先溶于水的氢氧化锂溶液(含氢氧化锂0.2g),温度控制在130 ℃,反应1 h。皂化结束后加入31.7 g PAO8,温度控制在200 ℃,持续10min后,停止加热。温度降到190 ℃时,加入31.7 g PAO8,体系降温至100 ℃时,停止搅拌,用三辊机研磨均匀后即得基础锂基润滑脂1。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.95 g 氯化镁、0.98 g 磷酸,0.53 g氯化铵在0.9 mL水溶液中反应。温度25 ℃,反应8天,经过滤、蒸馏水洗涤,室温干燥后即可获得无机铵插层型层状磷酸镁MgNH4PO4·H2O。
选用无机铵插层型层状磷酸镁MgNH4PO4·H2O1.0 g,2, 6-二叔丁基对甲苯酚0.05g与上述基础锂基润滑脂1 98.95 g在室温下搅拌10 h,利用三辊机研磨均化0.5 h使均匀,制得成品锂基润滑脂。
实施例 2
将23.3 g 100SN加入制脂釜中,启动搅拌器,加热升温至80 ℃,投入30.0 g硬脂酸,待硬脂酸完全溶解,再加入预先溶于水的氢氧化锂溶液(含氢氧化锂3.0 g),温度控制在120 ℃,反应5 h。皂化结束后加入23.3 g 100 SN,温度控制在220 ℃,持续10 min后,停止加热。温度降到160 ℃时,加入23.3 g 100 SN,体系降温至100 ℃时,停止搅拌,用高压均质机研磨均匀后即得基础锂基润滑脂2。
在30 mL聚四氟乙烯不锈钢釜中加入原料醋酸镁0.43 g、1.96 g 磷酸,1.2 g尿素在3.6 mL水溶液中反应。温度300 ℃,反应0.1天,经过滤、蒸馏水洗涤,室温干燥后即可获得无机铵插层型层状磷酸镁MgNH4PO4·H2O。
选用无机铵插层型层状磷酸镁MgNH4PO4·H2O10.0 g,β-萘酚5.0 g,烯基丁二酸6.0 g与上述基础锂基润滑脂2 79.0 g在200 ℃下搅拌混合1 h,利用高压均质机均化3 h使均匀,制得成品锂基润滑脂。
实施例 3
将30.0 g二甲基硅油倒入制脂釜中,启动搅拌器,加热升温至75 ℃,投入10.0 g硬脂酸,待硬脂酸完全溶解,再加入预先溶于水的氢氧化锂溶液(含氢氧化锂2.1 g),温度控制在125 ℃,反应3 h。皂化结束后加入30.0 g二甲基硅油,温度控制在210 ℃,持续10min后,停止加热。温度降到180 ℃时,加入30.0 g二甲基硅油,体系降温至100 ℃时,停止搅拌,用三辊机研磨均匀后即得基础锂基润滑脂3。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.63 g 无定型磷酸镁、0.59 g 磷酸和0.54 g 乙二胺,在1.6 mL水中反应。温度100 ℃,反应6天,经过滤、蒸馏水洗涤,室温干燥后即可获得乙二胺插层型层状磷酸镁MgP-EDA。
选用乙二胺插层型层状磷酸镁MgP-EDA 2.0 g,二苯胺1.0 g,十二烯基丁二胺2.0g与上述基础锂基润滑脂3 95.0 g在180 ℃下搅拌混合2 h,利用三辊机研磨均化2 h使均匀,制得成品锂基润滑脂。
实施例 4
将30.0 g二甲基硅油和60.0 g PAO8 混合均匀,将30.0 g 混合油样倒入制脂釜中,启动搅拌器,加热升温至76 ℃,投入15.0 g硬脂酸,待硬脂酸完全溶解,再加入预先溶于水的氢氧化锂溶液(含氢氧化锂1.8 g),温度控制在128 ℃,反应2 h。皂化结束后加入30.0 g混合油样,温度控制在215 ℃,持续10 min后,停止加热。温度降到175 ℃时,加入30.0 g混合油样,体系降温至100 ℃时,停止搅拌,用三辊机研磨均匀后即得基础锂基润滑脂3。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.42 g 无定型磷酸镁、0.78 g 磷酸和0.48 g 乙二胺,在1.0 mL水中反应。温度100 ℃,反应6天,经过滤、蒸馏水洗涤,室温干燥后即可获得乙二胺插层型层状磷酸镁MgP-EDA。
选用乙二胺插层型层状磷酸镁MgP-EDA 2.0 g,二苯胺1.0 g,十二烯基丁二胺2.0g与上述基础锂基润滑脂3 95.0 g在180 ℃下搅拌混合2 h,利用三辊机研磨均化2 h使均匀,制得成品锂基润滑脂。
实施例 5
制脂釜中加入27 g 季戊四醇酯,10.0 g硬脂酸,升温熔化,慢慢加入氢氧化锂水溶液(含氢氧化锂2.0 g),温度为115 ℃。加完氢氧化锂溶液后,温度迅速升至180 ℃,使皂基脱水完全,物料快冷至115 ℃,加入5.0 g己二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂2.0 g),使己二酸皂化,温度升至180 ℃保持1 h使脱水完全,迅速升温至220℃并保持20 min,加入54 g季戊四醇酯,使脂基迅速冷却,继续搅拌冷却至66 ℃,用三辊机研磨均匀后即得基础复合锂基润滑脂1。
在30 mL聚四氟乙烯不锈钢釜中加入原料1.9 g 氯化镁、9.8 g 磷酸和7.6 g 1,3-丙二胺,在10.8 mL水中反应。温度150 ℃,反应4天,经过滤、蒸馏水洗涤,室温干燥后即可获得1,3-丙二胺插层型层状磷酸镁MgP-PDA。
选用1,3-丙二胺插层型层状磷酸镁MgP-PDA 4.0 g,吩噻嗪3.0 g,苯并三氮唑2.0g与上述基础复合锂基润滑脂1 91.0 g在150 ℃下搅拌混合3 h,利用高压均质机均化1 h使均匀,制得成品复合锂基润滑脂。
实施例 6
制脂釜中加入31.3 g二羟甲基丙烷酯,4.0 g12-羟基硬脂酸,升温熔化,慢慢加入氢氧化锂水溶液(含氢氧化锂0.5 g),温度为80 ℃。加完氢氧化锂溶液后,温度迅速升至130 ℃,使皂基脱水完全,物料快冷至90 ℃,加入1.0 g壬二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂0.5 g),使壬二酸皂化,温度升至130 ℃保持1 h使脱水完全,迅速升温至200 ℃并保持20 min,加入62.6 g 二羟甲基丙烷酯,使脂基迅速冷却,继续搅拌冷却至66 ℃,用高压均质机研磨均匀后即得基础复合锂基润滑脂2。
在30 mL聚四氟乙烯不锈钢釜中加入原料2.09 g 无定型磷酸镁、5.28 g 1,4-丁二胺和5.88 g 磷酸,在9.0 mL水中反应。温度250 ℃,反应1天,经过滤、蒸馏水洗涤,室温干燥后即可获得1,4-丁二胺插层型层状磷酸镁MgP-DAB。
选用1,4-丁二胺插层型层状磷酸镁MgP-DAB 6.0 g,二苯胺2.0 g,烯基丁二酸1.0g与上述基础复合锂基润滑脂2 91.0 g在100 ℃下搅拌混合4 h,利用三辊机研磨均化3 h使均匀,制得成品复合锂基润滑脂。
实施例 7
制脂釜中加入30.0 g 液体石蜡,4.0 g12-羟基硬脂酸,升温熔化,慢慢加入氢氧化锂水溶液(含氢氧化锂1.0 g),温度为100 ℃。加完氢氧化锂溶液后,温度迅速升至150℃,使皂基脱水完全,物料快冷至105 ℃,加入4.0 g癸二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂1.0 g),使癸二酸皂化,温度升至150 ℃保持1 h使脱水完全,迅速升温至210 ℃并保持20 min,加入60.0 g 液体石蜡,使脂基迅速冷却,继续搅拌冷却至66℃,用高压均质机研磨均匀后即得基础复合锂基润滑脂3。
在30 mL聚四氟乙烯不锈钢釜中加入原料2.14 g 醋酸镁、8.12 g 1,6-己二胺和7.84 g 磷酸,在12.6 mL水中反应。温度180 ℃,反应2天,经过滤、蒸馏水洗涤,室温干燥后即可获得1,6-己二胺插层型层状磷酸镁MgP-HMD。
选用1,6-己二胺插层型层状磷酸镁MgP-HMD 8.0 g,吩噻嗪0.5 g与上述基础复合锂基润滑脂3 91.5 g在室温150 ℃下搅拌混合2 h,利用高压均质机均化2 h使均匀,制得成品复合锂基润滑脂。
实施例 8
将45.0 g 500 SN和45.0 g液体石蜡混合均匀,在制脂釜中加入30.0 g混合油样,6.0 g12-羟基硬脂酸,升温熔化,慢慢加入氢氧化锂水溶液(含氢氧化锂1.5 g),温度为105℃。加完氢氧化锂溶液后,温度迅速升至155 ℃,使皂基脱水完全,物料快冷至105 ℃,加入3.0 g癸二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂1.5 g),使癸二酸皂化,温度升至160 ℃保持1 h使脱水完全,迅速升温至215 ℃并保持20 min,加入60.0 g混合油样,使脂基迅速冷却,继续搅拌冷却至66 ℃,用高压均质机研磨均匀后即得基础复合锂基润滑脂4。
在30 mL聚四氟乙烯不锈钢釜中加入原料1.07 g 醋酸镁、5.22 g 1,6-己二胺和4.41 g 磷酸,在8.1 mL水中反应。温度180 ℃,反应2天,经过滤、蒸馏水洗涤,室温干燥后即可获得1,6-己二胺插层型层状磷酸镁MgP-HMD。
选用1,6-己二胺插层型层状磷酸镁MgP-HMD 8.0 g,吩噻嗪0.5 g与上述基础复合锂基润滑脂3 91.5 g在室温150 ℃下搅拌混合2 h,利用高压均质机均化2 h使均匀,制得成品复合锂基润滑脂。
为了进行对比,在每个实施例中,采用实施例中制备而成的基础锂基润滑脂或基础复合锂基润滑脂分别与石墨或MoS2复合,然后测试了性能。
利用四球摩擦磨损试验机对所制得润滑脂产品进行润滑性质评价实验,方法依据GB/T 3142-82和SH/T 0204-92。实验结果表明,添加插层型层状磷酸镁后,承载能力P B值显著提升,磨斑直径(WSD)明显减小,摩擦系数(µ)明显降低。具体的四球摩擦磨损试验结果数据如表1~8所示。
表1
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表2
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表3
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表4
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表5
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表6
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表7
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表8
Figure 247235DEST_PATH_IMAGE008
通过以上数据可以看出:与现有技术相比,承载能力P B值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。说明添加插层型层状磷酸镁材料到基础锂基脂中后,可有效提升润滑脂的承载、抗磨、减摩能力。

Claims (10)

1.以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:由以下重量份数的组分组成:
基础润滑脂79 - 98.95份,插层型层状磷酸镁材料1.0 - 10.0份,抗氧剂0.05 - 5.0份,防锈剂0 - 6.0份;
所述的基础润滑脂包括基础锂基润滑脂或基础复合锂基润滑脂;
所述的插层型层状磷酸镁材料为无机铵根插层型层镁MgNH4PO4·H2O,或有机胺插层型层镁0.5·[NH3(CH2)2NH3]2+·[MgPO4·H2O]- (MgP-EDA)、0.5·[NH3(CH2)3NH3]2+·[MgPO4·H2O]- (MgP-PDA)、0.5·[NH3(CH2)4NH3]2+·[MgPO4·H2O]- (MgP-DAB)或0.5·[NH3(CH2)6NH3]2+·[MgPO4·H2O]- (MgP-HMD)中的一种;
所述无机铵根插层型层镁的制备方法是将原料镁源、磷酸、无机铵盐在水溶液中反应,反应温度为25 - 300 ℃,反应时间0.1 - 8天,经过滤、蒸馏水洗涤,室温干燥后获得;
有机胺插层型层镁的制备方法是将原料镁源、磷酸、有机胺在水溶液中反应,反应温度为25 - 250 ℃,反应0.1 - 8天,经过滤、蒸馏水洗涤,室温干燥后获得。
2.根据权利要求1所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:由以下重量份数的组分组成:
基础润滑脂85 - 95份,插层型层状磷酸镁材料3.0 - 7.0份,抗氧剂0.05 - 3.0份,防锈剂0 - 4.0份;
所述的基础润滑脂包括基础锂基润滑脂或基础复合锂基润滑脂。
3.根据权利要求1所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:所述无机铵根插层型层镁的制备中,原料配比为磷镁摩尔比(1-10):1,铵镁摩尔比(1-10):1和水镁摩尔比(5-100):1;
所述无机铵盐为氯化铵、尿素、氨水中的一种;镁源为氯化镁、醋酸镁、无定型磷酸镁中的一种。
4.根据权利要求1所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:有机胺插层型层镁的制备中,原料配比为磷镁摩尔比(1-10):1,胺镁摩尔比(1-10):1和水镁摩尔比(5-100):1;
有机胺为乙二胺、1,3-丙二胺、1,4-丁二胺、1,6-己二胺中的一种;镁源为氯化镁、醋酸镁、无定型磷酸镁中的一种。
5.根据权利要求1所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:所述的抗氧剂包括2, 6-二叔丁基对甲苯酚、β-萘酚、二苯胺、吩噻嗪中的一种;所述的防锈剂包括烯基丁二酸、十二烯基丁二胺、苯并三氮唑中的一种。
6.根据权利要求1所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:
所述的基础锂基润滑脂是由原料脂肪酸、基础油和氢氧化锂反应而成,其中脂肪酸4.0- 30.0 份,基础油68.0 - 95.0 份,氢氧化锂0.2 - 3.0 份;
基础锂基润滑脂的制备方法:将1 / 3 基础油倒入制脂釜中,启动搅拌器,加热升温至70 - 80 ℃,投入脂肪酸,待脂肪酸完全溶解,再加入预先溶于水的氢氧化锂溶液,温度控制在120 - 130 ℃之间,反应1 - 5 h;皂化结束后加入1 / 3基础油,温度控制在200 -220 ℃之间,持续10 min后,停止加热;温度降到160 - 190 ℃时,加入1 / 3 基础油,体系降温至100 ℃时,停止搅拌,用三辊机或高压均质机研磨均匀后即得基础锂基润滑脂。
7.根据权利要求1所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:所述的基础复合锂基润滑脂是由包括脂肪酸、复合剂、氢氧化锂和基础油在内的原料混合而成,其中脂肪酸4.0 - 10.0份,复合剂1.0 - 5.0份,氢氧化锂1.0 - 4.0份,基础油81.0 - 94.0份;
基础复合锂基润滑脂的制备方法:向制脂釜中加入1 / 3 基础油,脂肪酸,升温熔化,慢慢加入1 / 2 的氢氧化锂水溶液,温度为80 - 115 ℃;
加完氢氧化锂溶液后,温度迅速升至130 - 180 ℃,使皂基脱水完全,物料快冷至90 -115 ℃,加入复合剂,搅拌10 min,慢慢加入1/2 氢氧化锂水溶液,使复合剂皂化,温度升至130 - 180 ℃保持1 h 使脱水完全,迅速升温至200 - 220 ℃并保持20 min,加入2 / 3基础油,使脂基迅速冷却,继续搅拌冷却至66 ℃,用三辊机或高压均质机研磨均匀后即得基础复合锂基润滑脂。
8.根据权利要求6或7所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:所述的脂肪酸包括12-羟基硬脂酸或硬脂酸;所述的基础油选自烃类基础油、酯类基础油、硅油类基础油中的一种或几种,选取几种时以任意比混合。
9.根据权利要求7所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂,其特征在于:所述的复合剂为己二酸、辛二酸、癸二酸中的一种。
10.一种权利要求1~9任一项所述的以插层型层状磷酸镁作为固体润滑添加剂的润滑脂的制备方法,其特征在于:包括如下步骤:
将基础润滑脂、插层型层状磷酸镁材料、抗氧剂和防锈剂在室温~ 200 ℃下搅拌混合1- 10 h,利用三辊机或高压均质机研磨均化0.5 - 3 h使之均匀,制得润滑脂产品。
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