CN106978233A - 一种高温抗磨减摩复配添加剂及其应用 - Google Patents

一种高温抗磨减摩复配添加剂及其应用 Download PDF

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CN106978233A
CN106978233A CN201710225099.9A CN201710225099A CN106978233A CN 106978233 A CN106978233 A CN 106978233A CN 201710225099 A CN201710225099 A CN 201710225099A CN 106978233 A CN106978233 A CN 106978233A
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张松伟
胡丽天
李毅
丁奇
秦宝锋
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Lanzhou Institute of Chemical Physics LICP of CAS
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    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract

本发明公开了一种高温抗磨减摩复配添加剂，该复配添加剂由巯基苯并噻唑类功能化离子液体和聚乙烯吡咯烷酮表面修饰的金属钼纳米颗粒组成；巯基苯并噻唑类功能化离子液体和聚乙烯吡咯烷酮表面修饰的金属钼纳米颗粒的质量比为1:9~9:1；巯基苯并噻唑类功能化离子液体为MBTILs‑1或MBTILs‑2，其结构式如下：

Description

一种高温抗磨减摩复配添加剂及其应用
技术领域
本发明涉及一种高温抗磨减摩复配添加剂及其应用，该复配添加剂具有优异的抗磨减摩性能，含该复配添加剂的润滑剂组合物具有良好的高温润滑性能。
背景技术
离子液体兼具离子化合物和有机化合物的诸多优点，作为绿色化学介质在有机合成、催化、电化学、物质分离和表面活性剂等许多领域具有重要的应用。在润滑工程领域，离子液体作为润滑剂和添加剂的应用研究引起了国内外科学家的广泛关注，相关研究也越来越深入。与现役润滑油脂及添加剂相比，离子液体的优势主要表现在：（1）结构可设计性强；（2）挥发性能极低；（3）液程宽；（4）承载能力高；（5）几乎不可燃，安全性高；（6）导电性好，其不足主要表现为：摩擦降解或热解易产生腐蚀性酸，从而引起金属材料的腐蚀。尤其是在高温条件下，离子液体会对金属摩擦副造成严重的腐蚀及腐蚀磨损问题。因此，降低离子液体的腐蚀性，改善其对金属摩擦副的适用性，是润滑工程领域的热点研究问题。
金属纳米颗粒是一种独特的润滑油脂添加剂，与传统添加剂不同，它通常不与基底材料发生摩擦化学反应，而是在摩擦副表面形成一层金属边界保护膜，从而发挥降低摩擦和减小磨损的作用。这种“非牺牲性”的减摩抗磨机制使得金属纳米颗粒添加剂能够在降低摩擦系数的同时，有效地保护摩擦副，避免引起严重的磨损问题。金属纳米颗粒添加剂的这一特点就为解决离子液体对摩擦副材料的腐蚀性，改善其对金属摩擦副的润滑性能提供了一条可行的途径。
发明内容
本发明的目的在于提供一种高温抗磨减摩复配添加剂及其应用。
本发明将离子液体与金属纳米颗粒进行复配，通过调节二者配比，获得一种适用于高温条件下的减摩抗磨添加剂，提升了离子液体对金属摩擦副的适用性，拓展了离子液体在润滑工程领域的应用空间。
一种高温抗磨减摩复配添加剂，其特征在于该复配添加剂由巯基苯并噻唑类功能化离子液体（记作MBTILs）和聚乙烯吡咯烷酮表面修饰的金属钼纳米颗粒（记作n-Mo）组成；所述MBTILs和n-Mo的质量比为1:9~9:1；所述MBTILs为MBTILs-1或MBTILs-2，其结构式如下：
。
所述聚乙烯吡咯烷酮占n-Mo的质量百分含量＜3%。
所述n-Mo的粒径尺寸为20-60 nm。
所述MBTILs-1通过以下方法制备得到：首先，分别配制2-巯基苯并噻唑的甲醇溶液和氢氧化钾的甲醇溶液，然后，向氢氧化钾的甲醇溶液滴加2-巯基苯并噻唑的甲醇溶液，滴加完毕后在60-80 ℃条件下搅拌30-60 min，待反应溶液冷却至室温，加入十二烷基三甲基氯化铵，搅拌反应15-30 h，然后过滤，用甲醇洗涤，将滤液旋蒸除去溶剂，再经80-120 ℃真空干燥24-36 h，得到MBTILs-1。
所述2-巯基苯并噻唑与氢氧化钾的摩尔比为1：1。
所述2-巯基苯并噻唑与十二烷基三甲基氯化铵的摩尔比为1：1~1.13。
如上所述高温减摩抗磨复配添加剂的应用，其特征在于：将MBTILs-1或MBTILs-2加入聚乙二醇基础油中，经超声波分散1-6 min即可获得含MBTILs添加剂的润滑剂组合物，记作润滑剂组合物A；将n-Mo加入聚乙二醇基础油中，经超声波分散5-8 min即可获得含n-Mo添加剂的润滑剂组合物，记作润滑剂组合物B；将润滑剂组合物A与润滑剂组合物B等质量混合，经磁力搅拌1-5 min即可获得含高温减摩抗磨复配添加剂的润滑剂组合物，记作润滑剂组合物C。
所述润滑剂组合物C中MBTILs-1或MBTILs-2的质量分数为0.2-1.8%，n-Mo的质量分数为0.2-1.8%，聚乙二醇基础油的质量分数为98%。
所述聚乙二醇基础油为PEG200、PEG400、PEG600中的一种。
所述MBTILs-2按照CN201610771728.3的制备方法获得。
所述n-Mo表面的聚乙烯吡咯烷酮修饰，作用为提高纳米颗粒的稳定性及其在基础油中的分散性。
本发明获得的含高温减摩抗磨复配添加剂的润滑剂组合物具有良好的高温润滑性能，其具体测试方案通过以下步骤来完成：
在Optimol 公司SRV-IV 微振动摩擦磨损试验机上考察了含高温减摩抗磨复配添加剂的润滑剂组合物的摩擦学性能，并与含2%MBTILs或2%n-Mo的润滑剂组合物作对比。选定载荷100 N，温度100 ℃，频率25 Hz，振幅1 mm，实验时间60 min，实验上试球为Φ10 mm的AISI52100钢球，下试样为Φ24×8 mm的AISI52100样块。摩擦实验结束后，采用MicroXAM公司非接触式三维表面轮廓仪检测样块的磨损情况。实验结果表明，如表1、图1和图2所示，高温条件下，将MBTILs与n-Mo复配得到的复配添加剂表现出两种添加剂的协同效果，能够大幅改善基础油的摩擦学性能，表现出极低且平稳的摩擦系数和更小的磨损量，且表现出优于两种添加剂单剂的减摩抗磨效果。
表1 聚乙二醇基础油、含2%MBTILs的润滑剂组合物、含2%n-Mo的润滑剂组合物和含复配添加剂的润滑剂组合物作为钢/钢润滑剂的平均摩擦系数
附图说明
图1为聚乙二醇基础油、含2%MBTILs的润滑剂组合物、含2%n-Mo的润滑剂组合物和含复配添加剂的润滑剂组合物作为钢/钢润滑剂的实时摩擦系数比较图。
图2为聚乙二醇基础油、含2%MBTILs的润滑剂组合物、含2%n-Mo的润滑剂组合物和含复配添加剂的润滑剂组合物作为钢/钢润滑剂的体积磨损量比较图。
具体实施方式
下面通过具体实施例来说明本发明，其在于进一步描述而非限制本发明。
实施例1
将25.09 g 2-巯基苯并噻唑和8.42 g氢氧化钾分别溶解于60 mL甲醇中，然后将二者混合于装有冷凝管与温度计的250 mL三口圆底烧瓶中，40 ℃条件下，搅拌30 min，过程中溶液始终保持澄清透明。将溶液冷却至室温后，加入40.52 g十二烷基三甲基氯化铵，搅拌反应30h，过程中逐渐有沉淀生成。产物通过慢速滤纸过滤，用150mL甲醇分三次洗涤，将滤液旋蒸除去溶剂，再经80℃真空干燥24h得到MBTILs-1。
将1 g MBTILs-1加入49 g基础油PEG200中，经超声波分散3min即可获得50 g含MBTILs-1添加剂的润滑剂组合物，记作PEG200+2%MBTILs-1。再将1 g n-Mo加入49 g基础油PEG200中，经超声波分散8 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG200+2%n-Mo。然后，将50 g PEG200+2%MBTILs-1与50 g PEG200+2%n-Mo混合，经磁力搅拌4 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG200+1%MBTILs-1 +1%n-Mo。
实施例2
将25.09 g 2-巯基苯并噻唑和8.42 g氢氧化钾分别溶解于50 mL甲醇中，然后将二者混合于装有冷凝管与温度计的250 mL三口圆底烧瓶中，40 ℃条件下，搅拌50 min，过程中溶液始终保持澄清透明。将溶液冷却至室温后，加入41.58 g十二烷基三甲基氯化铵，搅拌反应24h，过程中逐渐有沉淀生成。产物通过慢速滤纸过滤，用150mL甲醇分三次洗涤，将滤液旋蒸除去溶剂，再经80℃真空干燥36h得到MBTILs-1。
将1.5 g MBTILs-1加入48.5 g基础油PEG200中，经超声波分散5 min即可获得50g含MBTILs-1添加剂的润滑剂组合物，记作PEG200+3%MBTILs-1。再将0.5 g n-Mo加入49.5g基础油PEG200中，经超声波分散6 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG200+1%n-Mo。然后，将50 g PEG200+3%MBTILs-1与50 g PEG200+1%n-Mo混合，经磁力搅拌3 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG200+1.5%MBTILs-1 +0.5%n-Mo。
实施例3
将41.81 g 2-巯基苯并噻唑和14.02 g氢氧化钾分别溶解于100 mL甲醇中，然后将二者混合于装有冷凝管与温度计的500 mL三口圆底烧瓶中，50 ℃条件下，搅拌40 min，过程中溶液始终保持澄清透明。将溶液冷却至室温后，加入68.87 g十二烷基三甲基氯化铵，搅拌反应30h，过程中逐渐有沉淀生成。产物通过慢速滤纸过滤，用150mL甲醇分三次洗涤，将滤液旋蒸除去溶剂，再经80℃真空干燥30h得到MBTILs-1。
将1 g MBTILs-1加入49 g基础油PEG400中，经超声波分散3min即可获得50 g含MBTILs-1添加剂的润滑剂组合物，记作PEG400+2%MBTILs-1。再将1 g n-Mo加入49 g基础油PEG400中，经超声波分散6 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG400+2%n-Mo。然后，将50 g PEG400+2%MBTILs-1与50 g PEG400+2%n-Mo混合，经磁力搅拌4 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG400+1%MBTILs-1 +1%n-Mo。
实施例4
将41.81 g 2-巯基苯并噻唑和14.02 g氢氧化钾分别溶解于100 mL甲醇中，然后将二者混合于装有冷凝管与温度计的500 mL三口圆底烧瓶中，50 ℃条件下，搅拌40 min，过程中溶液始终保持澄清透明。将溶液冷却至室温后，加入68.87 g十二烷基三甲基氯化铵，搅拌反应30h，过程中逐渐有沉淀生成。产物通过慢速滤纸过滤，用150mL甲醇分三次洗涤，将滤液旋蒸除去溶剂，再经80℃真空干燥30h得到MBTILs-1。
将1.5 g MBTILs-1加入48.5 g基础油PEG600中，经超声波分散5min即可获得50 g含MBTILs-1添加剂的润滑剂组合物，记作PEG600+3%MBTILs-1。再将0.5 g n-Mo加入49.5 g基础油PEG600中，经超声波分散6 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG600+1%n-Mo。然后，将50 g PEG600+3%MBTILs-1与50 g PEG600+1%n-Mo混合，经磁力搅拌5 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG600+1.5%MBTILs-1 +0.5%n-Mo。
实施例5
将1 g MBTILs-2加入49 g基础油PEG200中，经超声波分散3min即可获得50 g含MBTILs-2添加剂的润滑剂组合物，记作PEG200+2%MBTILs-2。再将1 g n-Mo加入49 g基础油PEG200中，经超声波分散8 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG200+2%n-Mo。然后，将50 g PEG200+2%MBTILs-2与50 g PEG200+2%n-Mo混合，经磁力搅拌4 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG200+1%MBTILs-2 +1%n-Mo。
实施例6
将1.5 g MBTILs-2加入48.5 g基础油PEG200中，经超声波分散5 min即可获得50 g含MBTILs-2添加剂的润滑剂组合物，记作PEG200+3%MBTILs-2。再将0.5 g n-Mo加入49.5 g基础油PEG200中，经超声波分散6 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG200+1%n-Mo。然后，将50 g PEG200+3%MBTILs-2与50 g PEG200+1%n-Mo混合，经磁力搅拌3 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG200+1.5%MBTILs-2 +0.5%n-Mo。
实施例7
将0.5 g MBTILs-2加入49.5 g基础油PEG400中，经超声波分散3min即可获得50 g含MBTILs-2添加剂的润滑剂组合物，记作PEG400+1%MBTILs-2。再将1.5 g n-Mo加入48.5 g基础油PEG400中，经超声波分散8 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG400+3%n-Mo。然后，将50 g PEG400+1%MBTILs-1与50 g PEG400+3%n-Mo混合，经磁力搅拌4 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG400+0.5%MBTILs-1 +1.5%n-Mo。
实施例8
将1.5 g MBTILs-2加入48.5 g基础油PEG600中，经超声波分散5min即可获得50 g含MBTILs-2添加剂的润滑剂组合物，记作PEG600+3%MBTILs-2。再将0.5 g n-Mo加入49.5 g基础油PEG600中，经超声波分散6 min即可获得含n-Mo添加剂的润滑剂组合物，记作PEG600+1%n-Mo。然后，将50 g PEG600+3%MBTILs-2与50 g PEG600+1%n-Mo混合，经磁力搅拌5 min即可获得100 g含高温减摩抗磨复配添加剂的润滑剂组合物，记作PEG600+1.5%MBTILs-2 +0.5%n-Mo。
对比实施例
按照实施例1和实施例2中方法，制备得到50 g PEG200+2%MBTILs-1，50 g PEG200+2%MBTILs-2和50 g PEG200+ 2%n-Mo，分别作为高温摩擦试验的对比样品。

Claims (9)

1.一种高温抗磨减摩复配添加剂，其特征在于该复配添加剂由巯基苯并噻唑类功能化离子液体和聚乙烯吡咯烷酮表面修饰的金属钼纳米颗粒组成；所述MBTILs和n-Mo的质量比为1:9~9:1；所述MBTILs为MBTILs-1或MBTILs-2，其结构式如下：
。
2.如权利要求1所述的复配添加剂，其特征在于所述聚乙烯吡咯烷酮占n-Mo的质量百分含量＜3%。
3.如权利要求1所述的复配添加剂，其特征在于所述n-Mo的粒径尺寸为20-60 nm。
4.如权利要求1所述的复配添加剂，其特征在于所述MBTILs-1通过以下方法制备得到：首先，分别配制2-巯基苯并噻唑的甲醇溶液和氢氧化钾的甲醇溶液，然后，向氢氧化钾的甲醇溶液滴加2-巯基苯并噻唑的甲醇溶液，滴加完毕后在60-80 ℃条件下搅拌30-60 min，待反应溶液冷却至室温，加入十二烷基三甲基氯化铵，搅拌反应15-30 h，然后过滤，用甲醇洗涤，将滤液旋蒸除去溶剂，再经80-120 ℃真空干燥24-36 h，得到MBTILs-1。
5.如权利要求4所述的复配添加剂，其特征在于所述2-巯基苯并噻唑与氢氧化钾的摩尔比为1：1。
6.如权利要求4所述的复配添加剂，其特征在于所述2-巯基苯并噻唑与十二烷基三甲基氯化铵的摩尔比为1：1~1.13。
7.如权利要求1至6中任一项所述高温减摩抗磨复配添加剂的应用，其特征在于：将MBTILs-1或MBTILs-2加入聚乙二醇基础油中，经超声波分散1-6 min即可获得含MBTILs添加剂的润滑剂组合物，记作润滑剂组合物A；将n-Mo加入聚乙二醇基础油中，经超声波分散5-8 min即可获得含n-Mo添加剂的润滑剂组合物，记作润滑剂组合物B；将润滑剂组合物A与润滑剂组合物B等质量混合，经磁力搅拌1-5 min即可获得含高温减摩抗磨复配添加剂的润滑剂组合物，记作润滑剂组合物C。
8.如权利要求7所述的应用，其特征在于所述润滑剂组合物C中MBTILs-1或MBTILs-2的质量分数为0.2-1.8%，n-Mo的质量分数为0.2-1.8%，聚乙二醇基础油的质量分数为98%。
9.如权利要求7所述的应用，其特征在于所述聚乙二醇基础油为PEG200、PEG400、PEG600中的一种。
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