CN107384559B - 一种层状磷酸钾镁钠基润滑脂组合物及其制备方法 - Google Patents

一种层状磷酸钾镁钠基润滑脂组合物及其制备方法 Download PDF

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CN107384559B
CN107384559B CN201710645565.9A CN201710645565A CN107384559B CN 107384559 B CN107384559 B CN 107384559B CN 201710645565 A CN201710645565 A CN 201710645565A CN 107384559 B CN107384559 B CN 107384559B
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sodium
potassium
magnesium phosphate
magnesium
lubricating grease
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CN107384559A (zh
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董晋湘
张效胜
牛文星
代莹静
徐红
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Taiyuan University of Technology
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Abstract

本发明公开了一种层状磷酸钾镁钠基润滑脂组合物及其制备方法。该组合物包括以下重量份数的组分：基础钠基润滑脂为90.0‑98.0份，固体润滑添加剂为2.0‑10.0份；其中的固体润滑添加剂为层状磷酸钾镁MgKPO4·H2O。制备方法为：将基础钠基润滑脂、层状磷酸钾镁MgKPO4·H2O在室温~150℃下搅拌混合1‑24h，利用三联辊机或五联辊机研磨均化0.5‑10.0h使之均匀，制得钠基润滑脂产品。本发明提供的含有层状磷酸钾镁MgKPO4·H2O作为固体润滑添加剂的钠基润滑脂具有优异的抗磨能力。

Description

一种层状磷酸钾镁钠基润滑脂组合物及其制备方法
技术领域
本发明一种抗磨性能优异的钠基润滑脂组合物及其制备方法，具体涉及一种含有层状磷酸钾镁作为固体润滑添加剂的钠基润滑脂组合物及其制备方法，属于润滑技术领域。
背景技术
钠基润滑脂一般是由天然动植物油脂钠皂和脂肪酸钠皂稠化基础油而制得，具有良好的热稳定性、胶体安定性和剪切安定性。钠基润滑脂由于自身优势，在特定领域，如纺织、造纸等机械轴承润滑场所得到广泛应用。随着现代工业的迅速发展，高温、高速、重载设备的大量使用，轴承、汽车、印染、矿山、冶金和宇航等工业部门出现越来越多更加苛刻的工况，特别是许多润滑部位都是一次性充脂，在运行过程中无法补充或更换，所以对润滑脂的抗磨性能提出更高的要求。在基础钠基润滑脂中加入抗磨添加剂（包括二硫化钼、石墨等无机层状化合物）是一项有效措施，但二硫化钼、石墨等经典固体抗磨剂在适用范围、原料成本等方面也存在很多不足之处，积极寻找新型固体抗磨材料具有重要的意义。
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抗磨添加剂二硫化钼、石墨类似的层状晶体结构，有望表现出良好的润滑性能。我国是世界上镁矿资源最富有的国家之一，可利用镁矿资源储量约占世界总储量的70 %。因此，镁产品在中国的生产具有良好的经济性和竞争性，大力发展镁产业具有明显的资源优势。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。层状磷酸钾镁MgKPO4·H2O是由MgO6八面体、PO4四面体层板构成，钾离子和水分子存在于层板间构成的一种无机层状磷酸镁化合物[G Jovanovski, S Pocev, B Kaitner. Bulletin of theChemists and Technologists of Macedonia, 1997, 16(1): 59 - 63]，目前尚未有该层状磷酸钾镁作为润滑脂固体抗磨添加剂的报道。
发明内容
本发明旨在提供一种具有优异抗磨性能的钠基润滑脂及其制备方法，其中的固体润滑添加剂为层状磷酸钾镁MgKPO4·H2O。
本发明钠基润滑脂的质量份数组成包括：钠基润滑脂为90.0 - 98.0 份，固体润滑添加剂为2.0 - 10.0 份；其中的固体润滑添加剂为层状磷酸钾镁MgKPO4·H2O。
本发明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、层状磷酸钾镁MgKPO4·H2O在室温 - 150 ℃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 - 10.0 h使之均匀，制得钠基润滑脂产品。采用四球摩擦磨损试验机进行润滑性质评价。
如上所述的基础钠基润滑脂包括脂肪酸、抗氧剂、防锈剂、极压剂、氢氧化钠和基础油原料反应、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 - 3.0 份，防锈剂0 - 5.0 份，极压剂0 - 5.0 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系类合成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。
如上所述的层状磷酸钾镁材料MgKPO4·H2O，制备方法是将原料镁源、磷源和无机钾盐在水溶液中反应。温度范围25 - 250 ℃，0.1 - 10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。
所述的镁源选自氯化镁、醋酸镁、硫酸镁、无定型磷酸镁中的一种。
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、醋酸钾、硫酸钾、氢氧化钾中的一种。
本发明的优点和有益效果如下：
(1) 本发明报道含有层状磷酸钾镁MgKPO4·H2O作为固体润滑添加剂的钠基润滑脂具有优异的抗磨能力。
(2) 本发明报道层状磷酸钾镁MgKPO4·H2O作为钠基润滑脂的固体润滑添加剂，原料来源丰富，可有效降低工业应用的成本。
(3) 本发明报道层状磷酸钾镁MgKPO4·H2O作为钠基润滑脂的固体润滑添加剂，制备方法简便易行，与传统润滑脂抗氧剂、防锈剂、极压剂相容性好，易于制备出工业级产品。
附图说明
图1为实施例1所得层状磷酸钾镁的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31.7g 100 SN，5.0 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100 ℃，皂化约4 h；温度升至150 ℃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 g 100 SN，继续加热升温至190 ℃，进行稠化，加入0.05 g 二苯胺、5.0 g 烯基丁二酸和0.5 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2.14 g 醋酸镁、1.36 g 磷酸二氢钾，在0.9 mL水溶液中反应。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镁MgKPO4·H2O。图1即为该产品的XRD图。
选用层状磷酸钾镁MgKPO4·H2O 2.0 g与上述基础钠基润滑脂98.0 g在150 ℃下搅拌1 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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
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实施例 2
向制脂釜中加入21.7 g PAO8，35.0 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63.3 gPAO8，继续加热升温至200 ℃，进行稠化，加入3.0 g吩噻嗪、0.1 g 十二烯基丁二胺和5.0g 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0.19 g 氯化镁、0.46 g 磷酸氢二钾、1.49 g 氯化钾和0.2 g 磷酸，在3.6 mL水中反应。温度25 ℃，反应10天，经过滤、蒸馏水洗涤，室温干燥后即可获得层状磷酸钾镁MgKPO4·H2O。
选用层状磷酸钾镁MgKPO4·H2O 10.0 g与上述基础钠基润滑脂90.0 g在室温下搅拌混合24 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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
Figure 744788DEST_PATH_IMAGE002
实施例 3
向制脂釜中加入30.0 g 二甲基硅油，10.0 g 12-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 %；然后徐徐加入60.0 g 二甲基硅油，继续加热升温至195 ℃，进行稠化，加入1.0 g β-萘酚、1.0 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8 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0.12 g 硫酸镁、2.28 g 磷酸氢二钾和0.35 g 硫酸钾，在2 mL水溶液中反应。温度150 ℃，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镁MgKPO4·H2O。
选用层状磷酸钾镁MgKPO4·H2O 5.0 g与上述基础钠基润滑脂95.0 g在100 ℃下搅拌12 h，利用三联辊机研磨均化12 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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
Figure 597206DEST_PATH_IMAGE003
实施例 4
向制脂釜中加入27.0 g 500 SN，19.0 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30 %），温度为88 ℃。加完氢氧化钠溶液后，温度控制在108 ℃，皂化约4 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0.18 %；然后徐徐加入81.0g 500 SN，继续加热升温至196 ℃，进行稠化，加入1.0 g 2, 6-二叔丁基对甲苯酚、2.0 g苯并三氮唑和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0.42 g 无定型磷酸镁、0.28 g 氢氧化钾和0.29 g 磷酸，在5 mL水中反应。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镁MgKPO4·H2O。
选用层状磷酸钾镁MgKPO4·H2O 6.0 g与上述基础钠基润滑脂94.0 g在90 ℃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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
Figure 413853DEST_PATH_IMAGE004
实施例 5
向制脂釜中加入31.0 g PAO10，7.0 g 12-羟基硬脂酸，升温熔化，慢慢加入10.0g 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107 ℃，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0.17 %；然后徐徐加入62.0 g PAO10，继续加热升温至198 ℃，进行稠化，加入2.0 g 二苯胺、1.0 g 十二烯基丁二胺和3.0 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E。
在30 mL聚四氟乙烯不锈钢釜中加入原料1.29 g 醋酸镁、1.09 g 磷酸二氢钾和0.98 g 醋酸钾，在10 mL水溶液中反应。温度200 ℃，反应1天，经过滤、蒸馏水洗涤，室温干燥后即可获得层状磷酸钾镁MgKPO4·H2O。
选用层状磷酸钾镁MgKPO4·H2O 3.0 g与上述基础钠基润滑脂97.0 g在80 ℃下搅拌10 h，利用五联辊机研磨均化4.5 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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
Figure 806657DEST_PATH_IMAGE005
实施例 6
向制脂釜中加入23.0 g 液体石蜡，31.0 g 硬脂酸，升温熔化，慢慢加入12.0 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107 ℃，皂化约3.5 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0.19 %；然后徐徐加入46.0 g 液体石蜡，继续加热升温至193 ℃，进行稠化，加入3.0 g 吩噻嗪，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1.9 g 氯化镁、9.12g 磷酸氢二钾和5.88 g 磷酸，在13 mL水中反应。温度200 ℃，反应1天，经过滤、蒸馏水洗涤，室温干燥后即可获得层状磷酸钾镁MgKPO4·H2O。
选用层状磷酸钾镁MgKPO4·H2O 2.5 g与上述基础钠基润滑脂97.5 g在50 ℃下搅拌混合16 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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
Figure 126779DEST_PATH_IMAGE006
实施例 7
将20.0 g 100 SN和70.0 g PAO8混合均匀，向制脂釜中加入30.0 g混合油样，15.0 g 12-羟基硬脂酸，升温熔化，慢慢加入20.0 g 氢氧化钠水溶液（浓度为25 %），温度为85 ℃。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0.18 %；然后徐徐加入60.0 g 混合油样，继续加热升温至159 ℃，进行稠化，加入0.5 g 二苯胺、2.0 g 烯基丁二酸和2.5 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。
在30 mL聚四氟乙烯不锈钢釜中加入原料0.95 g 氯化镁、2.72 g 磷酸二氢钾，在10 mL水溶液中反应。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镁MgKPO4·H2O。
选用层状磷酸钾镁MgKPO4·H2O 4.0 g与上述基础钠基润滑脂96.0 g在100 ℃下搅拌10 h，利用三联辊机研磨均化1.5 h使均匀，制得钠基润滑脂G。
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镁后，承载能力P B值显著提升，磨斑直径（WSD）明显减小。
Figure 350432DEST_PATH_IMAGE008
通过以上数据可以看出：承载能力P B值显著提升，磨斑直径（WSD）明显减小。说明添加磷酸钾镁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 (8)

1.一种层状磷酸钾镁钠基润滑脂组合物，其特征在于包括以下重量份数的组分：
基础钠基润滑脂为90.0 - 98.0 份，固体润滑添加剂为2.0 - 10.0 份；其中的固体润滑添加剂为层状磷酸钾镁MgKPO4·H2O；
所述的层状磷酸钾镁MgKPO4·H2O，制备方法是将原料镁源、磷源和无机钾盐在水溶液中反应，反应温度为25 - 250 ℃，反应0.1 - 10天，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；
所述镁源为氯化镁、醋酸镁、硫酸镁、无定型磷酸镁中的一种；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、醋酸钾、硫酸钾、氢氧化钾中的一种。
2.一种权利要求1所述的层状磷酸钾镁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、层状磷酸钾镁MgKPO4·H2O在室温~150 ℃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 - 10.0 h使之均匀，制得钠基润滑脂产品。
3.根据权利要求2所述的层状磷酸钾镁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包括脂肪酸、抗氧剂、防锈剂、极压剂、氢氧化钠和基础油原料反应、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 - 3.0 份，防锈剂0 - 5.0 份，极压剂0 - 5.0 份。
4.根据权利要求2所述的层状磷酸钾镁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。
5.根据权利要求4所述的层状磷酸钾镁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。
6.根据权利要求4所述的层状磷酸钾镁钠基润滑脂组合物的制备方法，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。
7.根据权利要求4所述的层状磷酸钾镁钠基润滑脂组合物的制备方法，其特征在于：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。
8.根据权利要求4所述的层状磷酸钾镁钠基润滑脂组合物的制备方法，其特征在于：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系类合成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。
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