CN107502417B - 一种层状磷酸钾钙钠基润滑脂组合物及其制备方法 - Google Patents
一种层状磷酸钾钙钠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钠基润滑脂组合物及其制备方法。该组合物包括下列重量份数的组分:基础钠基润滑脂为90.0‑99.0份,固体抗磨添加剂为1.0‑10.0份;其中的固体抗磨添加剂为层状磷酸钾钙CaKPO4·H2O。制备方法为:将基础钠基润滑脂、层状磷酸钾钙CaKPO4·H2O在室温‑200℃下搅拌混合1‑24 h,利用三联辊机或五联辊机研磨均化0.5‑6 h使之均匀,制得钠基润滑脂产品。
Description
技术领域
本发明一种抗磨性质优良的钠基润滑脂及其制备方法,具体涉及一种含有层状磷酸钾钙作为抗磨添加剂的钠基润滑脂及其制备方法,属于润滑技术领域。
背景技术
随着工业机械的现代化,高温润滑脂得到越来越广泛的应用,钠基润滑脂因为价格适中,性能优异(良好的热稳定性、胶体安定性和剪切安定性),在许多重要的润滑场所(纺织机械、造纸机械等)起到不容忽视的作用。润滑脂润滑作用的关键是减少机械的摩擦和磨损,提高机械的效率、降低能耗。抗磨剂作为现代润滑油脂中主要添加剂之一,在减少摩擦磨损方面发挥着关键作用。以具有层状晶体结构的石墨、二硫化钼作为代表的固体抗磨添加剂应用广泛,但在材料成本、外观等方面的一些缺陷,也在一定程度上限制了它们的适用范围。 因此开发含有新型优质固体抗磨添加剂的钠基润滑脂,以适应多种苛刻工况的需求势在必行。
实际机械运转工况中,固体抗磨剂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抗磨添加剂的报道。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具有优良抗磨性能的钠基润滑脂及其制备方法,其中的固体抗磨添加剂为层状磷酸钾钙CaKPO4·H2O。
本发明钠基润滑脂的质量份数组成包括:基础钠基润滑脂为90.0 - 99.0份,固体抗磨添加剂为1.0 - 10.0份;其中的固体抗磨添加剂为层状磷酸钾钙CaKPO4·H2O。
本发明钠基润滑脂的制备方法包括如下步骤:按照合适的质量份数组成,将基础钠基润滑脂、层状磷酸钾钙CaKPO4·H2O在室温~200 ℃下搅拌混合1 - 24 h,利用三联辊机或五联辊机研磨均化0.5 - 6 h使之均匀,制得钠基润滑脂产品。
如上所述的基础钠基润滑脂由包括脂肪酸、抗氧剂、防锈剂、极压剂、氢氧
化钠和基础油在内的原料混合反应而成,其中脂肪酸5.0- 35.0 份,基础油65.0- 95.0 份,氢氧化钠0.5 - 5.0 份,抗氧剂0.05 - 5.0 份,防锈剂0 - 6.0 份,极压剂0 -6.0 份。
基础钠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,慢慢加入氢氧化钠水溶液(浓度为20 - 35 %),温度为80 - 90 ℃。加完氢氧化钠溶液后,温度控制在100 - 110 ℃,皂化约3 - 4 h;温度升至150 - 170 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.15 - 0.2 %范围内;然后徐徐加入剩余的基础油,继续加热升温至190- 200 ℃,进行稠化,加入抗氧剂、防锈剂和极压剂,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温5 - 10 min。急冷至100 ℃附近使用三联辊机或五联辊机进行均化。
所述的脂肪酸为12-羟基硬脂酸或硬脂酸。
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。
所述的极压剂为二烷基二硫代磷酸锌ZDDP或硫化异丁烯T321。
所述的基础油选自烃类矿物基础油、PAO系列合成基础油和硅油系列基础油中的一种或几种,任意比混合。
如上所述的层状磷酸钾钙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、无机钾盐在水溶液中反应;温度范围25 - 300 ℃,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。
所述的钙源选自氯化钙、醋酸钙、氢氧化钙、硫酸钙、碳酸钙中的一种。
所述的磷源选自磷酸、磷酸二氢钾、磷酸氢二钾中的一种。
所述的无机钾盐选自氯化钾、硫酸钾、醋酸钾、氢氧化钾中的一种。
本发明的优点和有益效果如下:
(1) 本发明报道添加层状磷酸钾钙作为固体润滑添加剂的钠基润滑脂具有良好的承载抗磨能力,适合多种苛刻工况。
(2) 本发明报道添加层状磷酸钾钙作为固体润滑添加剂的钠基润滑脂的制备,原料来源丰富,可有效降低工业应用的成本。
(3) 本发明报道添加层状磷酸钾钙作为固体润滑添加剂的钠基润滑脂,层状磷酸钾钙与各传统润滑脂添加剂间相容性良好,制备方法简便易行,易于实现工业化。
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
向制脂釜中加入30.0 g 100SN,10.0 g 12-羟基硬脂酸,升温熔化,慢慢加入25.0g 氢氧化钠水溶液(浓度为20 %),温度为80 ℃。加完氢氧化钠溶液后,温度控制在110 ℃,皂化约3 h;温度升至170 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.2 %;然后徐徐加入60.0 g 100SN,继续加热升温至200 ℃,进行稠化,加入0.05 g 2, 6-二叔丁基对甲苯酚、6.0 g 烯基丁二酸和6.0 g T321,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温5 min。急冷至100 ℃附近使用三联辊机进行均化,制得基础钠基润滑脂A。
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0.9 mL水溶液中反应。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。图1即为该产品的XRD图。
选用层状磷酸钾钙CaKPO4·H2O 1.0 g与上述基础钠基润滑脂99.0 g在室温下搅拌24 h,利用三联辊机研磨均化0.5 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
实施例 2
向制脂釜中加入31.7 g PAO10,5.0 g 硬脂酸,升温熔化,慢慢加入2.5 g 氢氧化钠水溶液(浓度为20 %),温度为90 ℃。加完氢氧化钠溶液后,温度控制在100 ℃,皂化约4h;温度升至170 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.15 %;然后徐徐加入63.3 gPAO10,继续加热升温至190 ℃,进行稠化,加入5.0 g β-萘酚、1.0 g 十二烯基丁二和1.0g ZDDP,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温10 min。急冷至100℃附近使用五联辊机进行均化,制得基础钠基润滑脂B。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.16 g 醋酸钙、1.74 g 磷酸氢二钾和1.74 g 硫酸钾,在1.8 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层状磷酸钾钙CaKPO4·H2O。
选用层状磷酸钾钙CaKPO4·H2O 10.0 g与上述基础钠基润滑脂90.0 g在200 ℃下搅拌11 h,利用三联辊机研磨均化0.5 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
实施例 3
向制脂釜中加入21.7 g PAO8,35.0 g 12-羟基硬脂酸,升温熔化,慢慢加入8.0 g氢氧化钠水溶液(浓度为35 %),温度为85 ℃。加完氢氧化钠溶液后,温度控制在105 ℃,皂化约3.5 h;温度升至155 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.19 %范围内;然后徐徐加入63.3 g PAO8,继续加热升温至195 ℃,进行稠化,加入4.0 g 吩噻嗪、2.0 g 苯并三氮唑和1.0 g ZDDP,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温6 min。急冷至100 ℃附近使用三联辊机进行均化,制得基础钠基润滑脂C。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.37 g 氢氧化钙、1.36 g 磷酸二氢钾和1.4 g 氢氧化钾,在4.5 mL水溶液中反应。温度180 ℃,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。
选用层状磷酸钾钙CaKPO4·H2O 1.0 g与上述基础钠基润滑脂99.0 g在室温 ℃下搅拌24 h,利用五联辊机研磨均化6 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
实施例 4
向制脂釜中加入27.0 g 500SN,20.0 g 硬脂酸,升温熔化,慢慢加入10.0 g氢氧化钠水溶液(浓度为35 %),温度为88 ℃。加完氢氧化钠溶液后,温度控制在108 ℃,皂化约3 h;温度升至165 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.16 %范围内;然后徐徐加入54.0 g 500SN,继续加热升温至196 ℃,进行稠化,加入3.0 g 2, 6-二叔丁基对甲苯酚和3.0 g 十二烯基丁二胺,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温8min。急冷至100 ℃附近使用五联辊机进行均化,制得基础钠基润滑脂D。
在30 mL聚四氟乙烯不锈钢釜中加入原料1.36 g 硫酸钙、2.72 g 磷酸二氢钾和2.94 g 磷酸,在15 mL水中反应。温度250 ℃,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。
选用层状磷酸钾钙CaKPO4·H2O 4.0 g与上述基础钠基润滑脂96.0 g在150 ℃下搅拌混合6 h,利用五联辊机均化5 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
实施例 5
向制脂釜中加入29.0 g 二甲基硅油,13.0 g12-羟基硬脂酸,升温熔化,慢慢加入10.0 g氢氧化钠水溶液(浓度为25 %),温度为86 ℃。加完氢氧化钠溶液后,温度控制在104℃,皂化约4 h;温度升至160 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.16 %范围内;然后徐徐加入58.0 g 二甲基硅油,继续加热升温至192 ℃,进行稠化,加入4.0 g β-萘酚和3.0 g T321,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温7min。急冷至100 ℃附近使用三联辊机进行均化,制得基础钠基润滑脂E。
在30 mL聚四氟乙烯不锈钢釜中加入原料1.0 g 碳酸钙、3.73 g 氯化钾和4.9 g磷酸,在8.0 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。
选用层状磷酸钾钙CaKPO4·H2O 6.0 g与上述基础钠基润滑脂94.0 g在180 ℃下搅拌混合1 h,利用三联辊机均化3 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
实施例 6
向制脂釜中加入22.0 g液体石蜡,34.0 g 硬脂酸,升温熔化,慢慢加入15.0 g 氢氧化钠水溶液(浓度为32 %),温度为83 ℃。加完氢氧化钠溶液后,温度控制在103 ℃,皂化约3.8 h;温度升至165 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.19 %;然后徐徐加入66.0 g 液体石蜡,继续加热升温至199 ℃,进行稠化,加入5.0 g 二苯胺,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温9 min。急冷至100 ℃附近使用五联辊机进行均化,制得基础钠基润滑脂F。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.74 g 氢氧化钙、0.98 g 醋酸钾和4.9g 磷酸,在5 mL水中反应。温度180 ℃,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。
选用层状磷酸钾钙CaKPO4·H2O 2.0 g与上述基础钠基润滑脂98.0 g在100 ℃下搅拌混合16 h,利用五联辊机均化2 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
实施例 7
将30.0 g 500SN和57.0 g 液体石蜡混合均匀,向制脂釜中加入29.0 g 混合油样,硬脂酸,升温熔化,慢慢加入15.0 g氢氧化钠水溶液(浓度为30 %),温度为86 ℃。加完氢氧化钠溶液后,温度控制在103 ℃,皂化约3.5 h;温度升至163 ℃进行脱水,观察釜内物料逐渐变稠,呈现粘稠拉丝状的时候,说明水已经基本脱净;160 ℃时进行游离酸碱含量的测定,使其控制在0.17 %范围内;然后徐徐加入58.0 g 混合油样,继续加热升温至194 ℃,进行稠化,加入2.0 g 2, 6-二叔丁基对甲苯酚和3.0 g 十二烯基丁二胺,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温7 min。急冷至100 ℃附近使用五联辊机进行均化,制得基础钠基润滑脂G。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.27 g 硫酸钙、1.36 g 磷酸二氢钾和0.59 g 磷酸,在2 mL水中反应。温度250 ℃,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。
选用层状磷酸钾钙CaKPO4·H2O 4.0 g与上述基础钠基润滑脂96.0 g在150 ℃下搅拌混合6 h,利用五联辊机均化5 h使均匀,制得成品钠基润滑脂。
利用四球摩擦磨损试验机对制得的钠基润滑脂的承载抗磨性质进行评价,实验参数参考GB / T 3142-82和SH / T 0204-92,实验结果表明添加层状磷酸钾钙后,承载能力P B值显著提升,磨斑直径(WSD)明显减小。
通过以上数据可以看出:与现有技术相比,本发明添加了层状磷酸钾钙CaKPO4·H2O的润滑脂,其承载能力P B值显著提升,磨斑直径(WSD)明显减小。说明添加磷酸钾钙材料到基础钠基脂中后,可有效提升润滑脂的承载、抗磨能力。
Claims (6)
1.一种层状磷酸钾钙钠基润滑脂组合物,其特征在于:包括下列重量份数的组分:
基础钠基润滑脂为90.0 - 99.0份,固体抗磨添加剂为1.0 - 10.0份;其中的固体抗磨添加剂为层状磷酸钾钙CaKPO4·H2O;
所述的层状磷酸钾钙CaKPO4·H2O制备方法采用水热合成方法,具体是将原料钙源、磷源、无机钾盐在水溶液中反应,反应温度为25 - 300 ℃,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所述的层状磷酸钾钙钠基润滑脂组合物,其特征在于:所述钙源为氯化钙、醋酸钙、氢氧化钙、硫酸钙、碳酸钙中的一种;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、氢氧化钾中的一种。
3.一种权利要求1~2任一项所述的层状磷酸钾钙钠基润滑脂组合物的制备方法,其特征在于:包括如下步骤:将基础钠基润滑脂、层状磷酸钾钙CaKPO4·H2O在室温~200 ℃下搅拌混合1 - 24 h,利用三联辊机或五联辊机研磨均化0.5 - 6 h使之均匀,制得钠基润滑脂产品。
4.根据权利要求3所述的层状磷酸钾钙钠基润滑脂组合物的制备方法,其特征在于:所述的基础钠基润滑脂是由包括脂肪酸、抗氧剂、防锈剂、极压剂、氢氧化钠和基础油在内的原料反应、混合而成,其中脂肪酸5.0 - 35.0 份,基础油65.0 - 95.0 份,氢氧化钠0.5 -5.0 份,抗氧剂0.05 - 5.0 份,防锈剂0 - 6.0 份,极压剂0 - 6.0 份。
5.根据权利要求3所述的层状磷酸钾钙钠基润滑脂组合物的制备方法,其特征在于:基础钠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,慢慢加入浓度为20 - 35 %的氢氧化钠水溶液,温度为80 - 90 ℃;加完氢氧化钠水溶液后,温度控制在100 - 110 ℃,皂化3 - 4 h;温度升至150 - 170 ℃进行脱水,观察釜内物料逐渐变稠;160 ℃时进行游离酸碱含量的测定,使其控制在0.15 - 0.2 %范围内;然后缓慢加入剩余的基础油,继续加热升温至190 - 200 ℃,进行稠化,加入抗氧剂、防锈剂和极压剂,继续升温至最高炼制温度,当釜内物料成真溶液状态后,保温5 - 10 min;急冷至100 ℃附近使用三联辊机或五联辊机进行均化。
6.根据权利要求5所述的层状磷酸钾钙钠基润滑脂组合物的制备方法,其特征在于:所述的脂肪酸为12-羟基硬脂酸或硬脂酸;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、苯并三氮唑的一种;所述的极压剂为二烷基二硫代磷酸锌ZDDP或硫化异丁烯T321;所述的基础油选自烃类矿物基础油、PAO系列合成基础油和硅油系列基础油中的一种或几种,选取几种时以任意比混合。
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