CN107502422B - 一种层状磷酸钾钙复合锂基润滑脂组合物及其制备方法 - Google Patents
一种层状磷酸钾钙复合锂基润滑脂组合物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种层状磷酸钾钙复合锂基润滑脂组合物及其制备方法。该组合物由以下重量份数的组分组成:基础复合锂基润滑脂74.0‑98.95份,层状磷酸钾钙CaKPO4·H2O1.0‑10.0份,抗氧剂0.05‑5.0份,防锈剂0‑6.0份,极压剂0‑5.0份。制备方法为:将基础复合锂基润滑脂、层状磷酸钾钙CaKPO4·H2O、抗氧剂、防锈剂和极压剂在室温~250℃下搅拌混合1‑12h,利用三辊机或高压均质机研磨均化0.5‑3 h使之均匀,制得复合锂基润滑脂组合物。本发明提供的层状磷酸钾钙CaKPO4·H2O为固体润滑添加剂的复合锂基润滑脂具有良好的极压承载抗磨减摩能力。
Description
技术领域
本发明涉及一种抗磨性能优异的复合锂基润滑脂、润滑脂固体润滑添加剂及其制备方法,属于润滑脂及其添加剂制备技术领域,具体涉及一种含有层状磷酸钾钙CaKPO4·H2O作为固体润滑添加剂的复合锂基润滑脂及其制备方法。
背景技术
润滑脂是工业领域中不可忽视的一种重要材料。我国现阶段经济飞速发展,工业上采用了许多大型重载机械、精密电子设备,这些设备许多部件都需要用到润滑脂。合适的润滑脂可有效地降低机械、电子设备的磨损,提高运行效率,降低运行能耗,是一种具有“节能降耗”特点的功能性精细化学品。随着经济的发展,对润滑脂性能的要求不断提高,以复合锂基润滑脂为代表的高滴点润滑脂有了很大的发展。目前,复合锂基润滑脂是我国润滑脂产品发展的一个主流品种。一般情况下,为了满足设备长期、稳定运转的需要,润滑脂需要添加固体润滑添加剂。
实际机械运转工况中,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。钙是地壳中分布最广泛的元素之一,占第五位,质量百分含量达到3.64 %。层状磷酸钾钙CaKPO4·H2O,具有与二硫化钼、石墨类似的层状晶体结构,有望表现出良好的润滑性能,目前尚未有该层状磷酸钾钙材料作为固体润滑添加剂的报道。在实际应用过程中,对固体润滑材料的物理化学性质(如纯度、粒径大小与分布、形貌等)是有要求的,矿物本身存在的杂质共生问题,会带来负面影响,利用人工合成的方法可有效解决这一问题,尚未有该层状磷酸钾钙矿物材料人工合成的报道。
发明内容
本发明旨在提供一种抗磨性能优异的复合锂基润滑脂、润滑脂固体润滑添加剂及其制备方法,其中的固体润滑添加剂为层状磷酸钾钙CaKPO4·H2O。
层状磷酸钾钙CaKPO4·H2O制备方法采用水热合成方法,具体来讲是将原料钙源、磷源、无机钾盐。温度范围25 - 250 ℃,0.1 - 7天进行反应,经过滤、蒸馏水洗涤,室温干燥后即可获得。原料的配比为磷镁摩尔比(1-10):1,钾镁摩尔比(1-10):1和水镁摩尔比(5-100):1。
如上所述的镁源选自氯化钙、醋酸钙、氢氧化钙、硫酸钙中的一种。
如上所述的磷源选自磷酸、磷酸二氢钾、磷酸氢二钾中的一种。
如上所述的无机钾盐选自氯化钾、硫酸钾、醋酸钾中的一种。
本发明提供了一种由上述润滑脂固体润滑添加剂制成的复合锂基润滑脂,润滑脂的质量份数组成为:基础复合锂基润滑脂74.0 - 98.95 份,层状磷酸钾钙CaKPO4·H2O 1.0- 10.0 份,抗氧剂0.05 - 5.0 份,防锈剂0 - 6.0 份,极压剂0 - 5.0 份。优选组成为:基础复合锂基润滑脂85.0 - 95.0 份,层状磷酸钾钙CaKPO4·H2O 3.0 - 8.0 份,抗氧剂0.5- 2.0 份,防锈剂0.5 - 2.0 份,极压剂1.0 - 3.0 份。
本发明复合锂基润滑脂的制备方法包括如下步骤:将基础复合锂基润滑脂、层状磷酸钾钙CaKPO4·H2O、抗氧剂、防锈剂和极压剂在室温 - 250 ℃下搅拌混合1 - 12 h,利用三辊机或高压均质机研磨均化0.5 - 3 h使之均匀,制得复合锂基润滑脂产品。
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混合、反应而成,其中脂肪酸4.0 - 10.0 wt.%,复合剂1.0 - 5.0 wt.%,氢氧化锂1.0 - 4.0 wt.%,基础油81.0 - 94.0 wt.%。
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 ℃,用三辊机研磨均匀后即得基础复合锂基润滑脂。
如上所述的脂肪酸包括12-羟基硬脂酸或硬脂酸。
如上所述的复合剂为己二酸、癸二酸、壬二酸。
如上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,选取几种时以任意比混合。
所述的烃类基础油是指PAO系列合成油、石蜡基矿物油、环烷基矿物油、中间基矿物油。
所述酯类基础油是指双酯油、多元醇酯油、复酯油或偏苯三酸酯油。
所述硅油类基础油是指甲基硅油、乙基硅油、甲苯基硅油或二苯基硅油。
如上所述的抗氧剂包括2, 6-二叔丁基对甲苯酚、吩噻嗪、二苯胺。
如上所述的防锈剂包括烯基丁二酸、苯并三氮唑。
如上所述的极压剂包括ZDDP、硫化异丁烯、磷酸三甲酚酯。
本发明的优点和有益效果如下:
(1)本发明首次采用水热合成方法,制备出层状磷酸钾钙CaKPO4·H2O,原料来源丰富,价格低廉,合成方法简便、条件温和,便于实现产品的质量控制。
(2)本发明报道含有层状磷酸钾钙CaKPO4·H2O作为固体润滑添加剂的复合锂基润滑脂中所含有的层状磷酸钾钙与常规润滑脂添加剂(抗氧剂、防锈剂、极压剂)配伍性良好。
(3)本发明报道层状磷酸钾钙CaKPO4·H2O为固体润滑添加剂的复合锂基润滑脂具有良好的极压承载抗磨减摩能力。
附图说明
图1为实施例1所得层状磷酸钾钙的XRD图。
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
在30 mL聚四氟乙烯不锈钢釜中加入原料:1.11 g 氯化钙、1.74 g磷酸氢二钾,在10 mL水溶液中反应。温度100 ℃,反应3天,经过滤、蒸馏水洗涤,室温干燥后即可获得层状磷酸钾钙CaKPO4·H2O。图1即为该产品的XRD图。
制脂釜中加入28.0 g PAO9,9.0 g 12-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170 ℃,使皂基脱水完全,物料快冷至105 ℃,加入4.0 g壬二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂1.5 g),使壬二酸皂化,温度升至170 ℃保持1 h使脱水完全,迅速升温至210 ℃并保持20 min,加入56.0 g PAO9,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。
选用层状磷酸钾钙CaKPO4·H2O 1.0 g,2, 6-二叔丁基对甲苯酚0.05 g与上述基础复合锂基润滑脂98.95 g在室温下搅拌12 h,利用三辊机研磨均化0.5 h使均匀,制得复合锂基润滑脂A。
利用四球摩擦磨损试验机,根据GB/T 3142-82和SH/T 0204-92评价复合锂基润滑脂的润滑性质,承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。
实施例 2
在30 mL聚四氟乙烯不锈钢釜中加入原料0.40 g 醋酸钙、1.86 g 氯化钾和2.45g 磷酸,在22.5 mL水中反应。温度150 ℃,反应2天,经过滤、蒸馏水洗涤,室温干燥后即可获得层状磷酸钾钙CaKPO4·H2O。
制脂釜中加入31.3 g 100 SN,4.0 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己二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂0.5 g),使己二酸皂化,温度升至130 ℃保持1 h使脱水完全,迅速升温至220 ℃并保持20 min,加入62.7 g 100 SN,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。
选用层状磷酸钾钙CaKPO4·H2O 10.0 g,二苯胺5.0 g,苯并三氮唑6.0 g,ZDDP5.0 g与上述基础复合锂基润滑脂74.0 g在室温250 ℃下搅拌混合1 h,利用三辊机均化3h使均匀,制得复合锂基润滑脂B。
利用四球摩擦磨损试验机,根据GB/T 3142-82和SH/T 0204-92评价复合锂基润滑脂的润滑性质,承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。
实施例 3
在30 mL聚四氟乙烯不锈钢釜中加入原料:2.72 g 硫酸钙、8.16 g 磷酸二氢钾和5.88 g 醋酸钾,在18 mL水中反应。温度25 ℃,反应7天,经过滤、蒸馏水洗涤,室温干燥后即可获得层状磷酸钾钙CaKPO4·H2O。
制脂釜中加入29.0 g 液体石蜡,8.0 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100 ℃,加入3.0 g己二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂1.0 g),使己二酸皂化,温度升至150 ℃保持1 h使脱水完全,迅速升温至205℃并保持20 min,加入58.0 g 液体石蜡,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。
选用层状磷酸钾钙CaKPO4·H2O 8.0 g,吩噻嗪3.0 g,烯烃丁二酸1.0 g,硫化异丁烯 1.0 g与上述基础复合锂基润滑脂87.0 g在50 ℃下搅拌混合2 h,利用三辊机研磨均化1 h使均匀,制得复合锂基润滑脂C。
利用四球摩擦磨损试验机,根据GB/T 3142-82和SH/T 0204-92评价复合锂基润滑脂的润滑性质,承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。
实施例 4
在30 mL聚四氟乙烯不锈钢釜中加入原料:3.16 g 醋酸钙、9.8 g 磷酸和10.44 g硫酸钾,在1.8 mL水中反应。温度250 ℃,反应0.1天,经过滤、蒸馏水洗涤,室温干燥后即可获得层状磷酸钾钙CaKPO4·H2O。
制脂釜中加入27.0 g 季戊四醇酯,10.0 g 12-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癸二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂2.0 g),使癸二酸皂化,温度升至180 ℃保持1 h使脱水完全,迅速升温至200 ℃并保持20 min,加入54.0 g 季戊四醇酯,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。
选用层状磷酸钾钙CaKPO4·H2O 5.0 g,吩噻嗪3.0 g,烯基丁二酸2.0 g,磷酸三甲酚酯2.0 g与上述基础复合锂基润滑脂88.0 g在100 ℃下搅拌混合3 h,利用高压均质机均化1 h使均匀,制得复合锂基润滑脂D。
利用四球摩擦磨损试验机,根据GB/T 3142-82和SH/T 0204-92评价复合锂基润滑脂的润滑性质,承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。
实施例 5
在30 mL聚四氟乙烯不锈钢釜中加入原料:0.74 g 氢氧化钙、2.94 g 醋酸钾和4.9 g 磷酸,在10 mL水中反应。温度100 ℃,反应5天,经过滤、蒸馏水洗涤,室温干燥后即可获得层状磷酸钾钙CaKPO4·H2O。
制脂釜中加入30.0 g 二甲基硅油,7.0 g 12-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95 ℃。加完氢氧化锂溶液后,温度迅速升至160℃,使皂基脱水完全,物料快冷至95 ℃,加入2.0 g 癸二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂0.5 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 二甲基硅油,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。
选用层状磷酸钾钙CaKPO4·H2O 3.0 g,二苯胺0.5 g,苯并三氮唑0.5 g,磷酸三甲酚酯1.0 g与上述基础复合锂基润滑脂95.0 g在200 ℃下搅拌混合4 h,利用三辊机研磨均化2 h使均匀,制得复合锂基润滑脂E。
利用四球摩擦磨损试验机,根据GB/T 3142-82和SH/T 0204-92评价复合锂基润滑脂的润滑性质,承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。
实施例 6
在30 mL聚四氟乙烯不锈钢釜中加入原料:0.56 g 氯化钙、0.75 g氯化钾和3.92g 磷酸,在15 mL水中反应。温度120 ℃,反应3天,经过滤、蒸馏水洗涤,室温干燥后即可获得层状磷酸钾钙CaKPO4·H2O。
将31 g PAO8和63 g 500 SN混合,先在制脂釜中加入31.3 g 混合油,4.0 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己二酸,搅拌10 min,慢慢加入氢氧化锂水溶液(含氢氧化锂0.5 g),使己二酸皂化,温度升至130 ℃保持1 h使脱水完全,迅速升温至220 ℃并保持20 min,加入62.7 g 混合油,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。
选用层状磷酸钾钙CaKPO4·H2O 8.0 g,二苯胺2.0 g,苯并三氮唑2.0 g,ZDDP 3.0g与上述基础复合锂基润滑脂85.0 g在室温250 ℃下搅拌混合1 h,利用三辊机均化3 h使均匀,制得复合锂基润滑脂F。
利用四球摩擦磨损试验机,根据GB/T 3142-82和SH/T 0204-92评价复合锂基润滑脂的润滑性质,承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。
通过以上数据可以看出:承载能力P B值和极压能力P D值显著提升,磨斑直径(WSD)和摩擦系数(µ)明显减小。说明添加磷酸钾钙材料到基础锂基脂中后,可有效提升润滑脂的极压、承载、抗磨、减摩能力。
Claims (8)
1.一种层状磷酸钾钙复合锂基润滑脂组合物,其特征在于:由以下重量份数的组分组成:
基础复合锂基润滑脂74.0 - 98.95 份,层状磷酸钾钙CaKPO4·H2O 1.0 - 10.0 份,抗氧剂0.05 - 5.0 份,防锈剂0 - 6.0 份,极压剂0 - 5.0 份;
所述层状磷酸钾钙CaKPO4·H2O的制备方法,具体是将原料钙源、磷源、无机钾盐在水溶液中反应;在温度为25 - 250 ℃,进行反应0.1 - 7天,经过滤、蒸馏水洗涤,室温干燥后获得层状磷酸钾钙CaKPO4·H2O;
原料的配比为磷钙摩尔比(1~10):1,钾钙摩尔比(1~10):1和水钙摩尔比(5-100):1。
2.根据权利要求1所述的磷酸钾钙复合锂基润滑脂组合物,其特征在于:由以下重量份数的组分组成:
基础复合锂基润滑脂85.0 - 95.0 份,层状磷酸钾钙CaKPO4·H2O 3.0 - 8.0 份,抗氧剂0.5 - 2.0 份,防锈剂0.5 - 2.0 份,极压剂1.0 - 3.0 份。
3.根据权利要求1所述的磷酸钾钙复合锂基润滑脂组合物,其特征在于:所述的抗氧剂包括2, 6-二叔丁基对甲苯酚、吩噻嗪、二苯胺中的一种;所述的防锈剂包括烯基丁二酸、苯并三氮唑中的一种;所述的极压剂包括ZDDP、硫化异丁烯、磷酸三甲酚酯中的一种。
4.根据权利要求1所述的磷酸钾钙复合锂基润滑脂组合物,其特征在于:所述钙源为氯化钙、醋酸钙、氢氧化钙、硫酸钙中的一种;磷源为磷酸、磷酸二氢钾、磷酸氢二钾中的一种;无机钾盐为氯化钾、硫酸钾中的一种。
5.一种权利要求1~4任一项所述的磷酸钾钙复合锂基润滑脂组合物的制备方法,其特征在于:包括如下步骤:将基础复合锂基润滑脂、层状磷酸钾钙CaKPO4·H2O、抗氧剂、防锈剂和极压剂在室温~250 ℃下搅拌混合1 - 12 h,利用三辊机或高压均质机研磨均化0.5 - 3h使之均匀,制得磷酸钾钙复合锂基润滑脂组合物。
6.根据权利要求5所述的磷酸钾钙复合锂基润滑脂组合物的制备方法,其特征在于:所述的基础复合锂基润滑脂由包括脂肪酸、复合剂、氢氧化锂和基础油在内的原料混合反应而成,其中脂肪酸4.0 - 10.0 wt.%,复合剂1.0 - 5.0 wt.%,氢氧化锂1.0 - 4.0 wt.%,基础油81.0 - 94.0 wt.%;
基础复合锂基润滑脂的制备方法为: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 ℃;加完氢氧化锂水溶液后,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10min,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 ℃,用三辊机研磨均匀后即得基础复合锂基润滑脂。
7.根据权利要求6所述的磷酸钾钙复合锂基润滑脂组合物的制备方法,其特征在于:所述的脂肪酸包括12-羟基硬脂酸或硬脂酸;所述的复合剂为己二酸、癸二酸、壬二酸中的任一种;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,选取几种时以任意比混合。
8.根据权利要求7所述的磷酸钾钙复合锂基润滑脂组合物的制备方法,其特征在于:所述的烃类基础油是指PAO系列合成油、石蜡基矿物油、环烷基矿物油、中间基矿物油中的一种;
所述酯类基础油是指双酯油、多元醇酯油、复酯油或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、甲苯基硅油或二苯基硅油中的一种。
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