CN110437924A - 一种无水皂化制备复合锂基润滑脂的方法 - Google Patents

一种无水皂化制备复合锂基润滑脂的方法 Download PDF

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CN110437924A
CN110437924A CN201910761980.XA CN201910761980A CN110437924A CN 110437924 A CN110437924 A CN 110437924A CN 201910761980 A CN201910761980 A CN 201910761980A CN 110437924 A CN110437924 A CN 110437924A
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周忠太
宋尚珍
齐瑞琴
李保莉
王利霞
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Xinxiang Hengxing Technology Co Ltd
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Abstract

本发明公开了一种无水皂化制备复合锂基润滑脂的方法，该复合锂基润滑脂由以下重量份的原料制得：基础油300‑600份、十二羟基硬脂酸32‑35份、硬脂酸4‑8份、甘油5‑6份、乙酸钠2‑3份、一水合氢氧化锂7‑9份、硼酸1.5‑2份、邻苯二甲酸异丙酯7‑10份、二苯胺1.5‑3份、二烷基二硫代氨基甲酸锑1.5‑3份和1‑1.5份苯并三氮唑。本发明制备的复合锂基润滑脂在热稳定性、胶体安定性、抗水性、机械安定性和抗极压能力各方面均表现优异，在本领域中处于上游水平。

Description

一种无水皂化制备复合锂基润滑脂的方法
技术领域
本发明属于复合锂基润滑脂的制备技术领域，具体涉及一种无水皂化制备复合锂基润滑脂的方法。
背景技术
锂基类润滑脂是当前最为主要、生产量最大、应用最为广泛、最受各国润滑脂行业重视的润滑脂类型之一。锂基润滑脂发展于20世纪40年代，由于具有良好的多效性能和较高的滴点，很快在各个领域取代其它润滑脂，并作为一种通用润滑脂广泛应用于飞机、坦克、舰船、汽车、冶金、造纸、纺织、食品器械以及仪表仪器、家用电器等领域。
锂基润滑脂的品种多，按照工艺来分，可分为通用锂基润滑脂和复合锂基润滑脂。通用锂基润滑脂一般用在汽车、挖掘设备以及一般的机械的设备例如机床等常温常压的轴承上。复合锂基润滑脂是在通用锂基润滑脂的工艺基础上增加了低分子二元酸进行复合，使锂基润滑脂的稠化剂纤维更加强韧，这样复合锂基润滑脂比通用锂基脂就有了更高的极压性能，更好的胶体安定性，更好的机械安定性能和更好的热稳定性，所以复合锂基润滑脂具有更好的应用前景和开发前景。
目前复合锂基润滑脂生产工艺中的第一步皂化反应都是在有机酸、氢氧化锂、水三者存在下进行。本发明是在无水参与的状态下，既能让体系皂化反应继续，同时又可以让低分子酸复合反应进行，两个反应同时进行，达到节省时间、节能、降低生产成本且提高产品性能的目的。
发明内容
本发明解决的技术问题是提供了一种无水皂化制备复合锂基润滑脂的方法，该方法突破了有水存在将反应温度限制在100℃左右的上限，可以让皂化反应进行的同时，使稠化剂之间的复合反应介入，缩短了生产时间，降低了能耗，提高了产品质量。
本发明为解决上述技术问题采用如下技术方案，一种无水皂化制备复合锂基润滑脂的方法，其特征在于具体步骤为：
步骤S1：将300-600重量份的基础油加入皂化釜中并升温至80℃，再将32-35重量份的十二羟基硬脂酸、4-8重量份的硬脂酸、5-6重量份的甘油、2-3重量份的乙酸钠、7-9重量份的一水合氢氧化锂和1.5-2重量份的硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕，所述基础油为石蜡基矿物油、环烷基矿物油或PA010合成油中的一种或多种，100℃时的运动粘度为10-15mm2/s，十二羟基硬脂酸的质量百分含量>95％，硬脂酸的质量百分含量>95％，甘油的质量百分含量>98％，乙酸钠的质量百分含量>99％,一水合氢氧化锂的质量百分含量>99％，硼酸的质量百分含量>99％，邻苯二甲酸异丙酯的质量百分含量>98％；
步骤S2：将皂化釜继续升温至150-160℃加入7-10重量份的邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入1.5-3重量份的二苯胺、1.5-3重量份的二烷基二硫代氨基甲酸锑和1-1.5重量份的苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂，所述二苯胺的质量百分含量>99％，二烷基二硫代氨基甲酸锑的质量百分含量>99％，苯并三氮唑的质量百分含量>99％。
本发明所述的无水皂化制备复合锂基润滑脂的方法，其特征在于具体步骤为：
步骤S1：将300重量份的石蜡基矿物油加入皂化釜中并升温至80℃，再将35重量份的十二羟基硬脂酸、5重量份的硬脂酸、5重量份的甘油、2重量份的乙酸钠、8重量份的一水合氢氧化锂和2重量份的硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕；
步骤S2：将皂化釜继续升温至150-160℃加入7重量份的邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入2重量份的二苯胺、2重量份的二烷基二硫代氨基甲酸锑和1重量份的苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂。
本发明制备的复合锂基润滑脂在热稳定性、胶体安定性、抗水性、机械安定性和抗极压能力各方面均表现优异，在本领域中处于上游水平。
本发明的突出特点就是无水皂化，但不是绝对的无水反应，反应过程中有水生成，但只是很微量的水。正是无水皂化使反应不再局限于100℃，而是可以通过提高反应复合的温度来改善润滑脂的成脂速度和成脂质量，同时也体现了节能和环保的理念。
通过实验对比，有水皂化和无水皂化反应所得的复合锂基润滑脂的颜色和透明度差距也比较明显，有水皂化的复合锂基润滑脂颜色较深，透明度差；无水皂化的复合锂基润滑脂即使反应中没有氮气保护，所得的复合锂基润滑脂的颜色与基础油颜色相近且透明度好。
具体实施方式
以下通过实施例对本发明的上述内容做进一步详细说明，但不应该将此理解为本发明上述主题的范围仅限于以下的实施例，凡基于本发明上述内容实现的技术均属于本发明的范围。
实施例1
步骤S1：将300千克石蜡基矿物油加入皂化釜中并升温至80℃，再将35千克十二羟基硬脂酸、5千克硬脂酸、5千克甘油、2千克乙酸钠、8千克一水合氢氧化锂和2千克硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕；
步骤S2：将皂化釜继续升温至150-160℃加入7千克邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入2千克二苯胺、2千克二烷基二硫代氨基甲酸锑和1千克苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂。
本实施例制得的复合锂基润滑脂的性能指标如下：
实施例2
步骤S1：将590千克石蜡基矿物油加入皂化釜中并升温至80℃，再将35千克十二羟基硬脂酸、5千克硬脂酸、5千克甘油、2千克乙酸钠、8.5千克一水合氢氧化锂和2千克硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕；
步骤S2：将皂化釜继续升温至150-160℃加入7千克邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入3千克二苯胺、3千克二烷基二硫代氨基甲酸锑和1.5千克苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂。
实施例3
步骤S1：将480千克石蜡基矿物油加入皂化釜中并升温至80℃，再将35千克十二羟基硬脂酸、5千克硬脂酸、5千克甘油、2千克乙酸钠、8千克一水合氢氧化锂和2千克硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕；
步骤S2：将皂化釜继续升温至150-160℃加入7千克邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入2千克二苯胺、2千克二烷基二硫代氨基甲酸锑和1.5千克苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂。
实施例4
步骤S1：将330千克石蜡基矿物油加入皂化釜中并升温至80℃，再将35千克十二羟基硬脂酸、5千克硬脂酸、5千克甘油、2千克乙酸钠、7.5千克一水合氢氧化锂和2千克硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕；
步骤S2：将皂化釜继续升温至150-160℃加入7千克邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入1.7千克二苯胺、1.7千克二烷基二硫代氨基甲酸锑和1千克苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂。
以上显示和描述了本发明的基本原理，主要特征和优点，在不脱离本发明精神和范围的前提下，本发明还有各种变化和改进，这些变化和改进都落入要求保护的本发明的范围。

Claims (2)

1.一种无水皂化制备复合锂基润滑脂的方法，其特征在于具体步骤为：
步骤S1：将300-600重量份的基础油加入皂化釜中并升温至80℃，再将32-35重量份的十二羟基硬脂酸、4-8重量份的硬脂酸、5-6重量份的甘油、2-3重量份的乙酸钠、7-9重量份的一水合氢氧化锂和1.5-2重量份的硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕，所述基础油为石蜡基矿物油、环烷基矿物油或PA010合成油中的一种或多种，100℃时的运动粘度为10-15mm2/s，十二羟基硬脂酸的质量百分含量>95%，硬脂酸的质量百分含量>95%，甘油的质量百分含量>98%，乙酸钠的质量百分含量>99%,一水合氢氧化锂的质量百分含量>99%，硼酸的质量百分含量>99%，邻苯二甲酸异丙酯的质量百分含量>98%；
步骤S2：将皂化釜继续升温至150-160℃加入7-10重量份的邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入1.5-3重量份的二苯胺、1.5-3重量份的二烷基二硫代氨基甲酸锑和1-1.5重量份的苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂，所述二苯胺的质量百分含量>99%，二烷基二硫代氨基甲酸锑的质量百分含量>99%，苯并三氮唑的质量百分含量>99%。
2.根据权利要求1所述的无水皂化制备复合锂基润滑脂的方法，其特征在于具体步骤为：
步骤S1：将300重量份的石蜡基矿物油加入皂化釜中并升温至80℃，再将35重量份的十二羟基硬脂酸、5重量份的硬脂酸、5重量份的甘油、2重量份的乙酸钠、8重量份的一水合氢氧化锂和2重量份的硼酸投入皂化釜中，搅拌升温至120-125℃恒温反应2-2.5h，硼酸复合完毕；
步骤S2：将皂化釜继续升温至150-160℃加入7重量份的邻苯二甲酸异丙酯进行复合反应1-1.5h，邻苯二甲酸异丙酯复合完毕；
步骤S3：将皂化釜继续升温至230-235℃进行高温炼制，恒温10min，整个皂化反应结束，将润滑脂转移至调和釜，待温度降温至90-110℃时加入2重量份的二苯胺、2重量份的二烷基二硫代氨基甲酸锑和1重量份的苯并三氮唑，经剪切、研磨、过滤、出脂包装即得复合锂基润滑脂。
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