CN114561237B - 一种剪切响应性水基凝胶润滑剂的制备方法 - Google Patents

一种剪切响应性水基凝胶润滑剂的制备方法 Download PDF

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CN114561237B
CN114561237B CN202210407670.XA CN202210407670A CN114561237B CN 114561237 B CN114561237 B CN 114561237B CN 202210407670 A CN202210407670 A CN 202210407670A CN 114561237 B CN114561237 B CN 114561237B
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胡丽天
曹文辉
丁奇
秦宝锋
张松伟
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

本发明公开了一种剪切响应性水基凝胶润滑剂的制备方法，是将丙烯酰胺、丙烯酸溶解于水中，加热搅拌至溶液澄清透明；向体系中通入高纯氮气并升温至70℃~75℃，加入交联剂MBA搅拌反应一段时间后，再加入引发剂APS聚合6~8h，得到该剪切响应性水基凝胶润滑剂溶液。该水基凝胶润滑剂初始为液态，容易注入摩擦界面；具有快速剪切响应特性，在摩擦过程中迅速增稠，在摩擦界面上形成润滑膜，具有优异的粘附能力。用于摩擦配副时，不但能降低摩擦系数，而且能极大缓解摩擦界面的粘着磨损。另外，该剪切响应水基凝胶润滑剂对于不同摩擦速度具有响应性，表现为在不同剪切速度下有着不同的摩擦系数，因此具有一定工况自适应特性。

Description

一种剪切响应性水基凝胶润滑剂的制备方法
技术领域
本发明涉及一种水基凝胶润滑剂的制备方法，尤其涉及一种剪切响应性水基凝胶润滑剂的制备方法，主要用于钢和氮化硅摩擦副的润滑，属于高分子材料领域和润滑技术领域。
技术背景
水润滑具有无污染、冷却性好、高安全性等特点，被广泛用于机械润滑、切削等领域。但由于水的黏度低、润滑过程中易流失、实际润滑效果比油润滑差等缺点限制了其使用范围。为了提高水的润滑性能，多种水溶性纳米颗粒被引入水润滑中，来降低摩擦副的摩擦磨损。近年来，软物质（聚合物刷、水凝胶）得到了广泛研究，特别是水凝胶这种亲水性三维网络结构材料，具有良好的生物相容性，而且其化学网络结构具有高度可设计性，各种响应性分子可被引入水凝胶网络中，可以通过改变外界环境达到凝胶体系中分子构象的转变，从而使得水凝胶对于不同的环境刺激能做出响应。目前研究广泛的有温度、pH、光、电等响应性水凝胶，已被广泛应用于药物释放、人工肌肉等领域。
随着摩擦学领域润滑自适应这一概念的提出，将响应性凝胶用于摩擦学领域的研究也逐渐得到了关注，但是水凝胶的机械强度普遍较弱，难以适应摩擦过程中的持续剪切。中国专利CN109825269A公开了一种剪切响应型凝胶堵漏剂在钻井液堵漏领域的应用，但该方案最终得到的是剪切变稀、静置增稠特性的剪切响应性凝胶；中国专利CN114058029A公开了一种震荡成胶技术，所制备的水凝胶原液轻微震荡后即可成胶，这并不适用于所需要的摩擦初始润滑剂容易注入、摩擦过程中具有剪切成胶这一工况自适应场景。因此，目前针对水润滑摩擦副，尚无具备剪切成胶和剪切增稠调控性能的水润滑技术方案。
发明内容
本发明的目的是针对现有水润滑技术中摩擦界面水润滑膜形成能力不足、易发生粘着磨损等问题，提供一种具有剪切响应性的高分子水基凝胶润滑剂的制备方法。
本发明公开的一种剪切响应性水基凝胶润滑剂的制备方法，是将丙烯酰胺（AM）、丙烯酸（AA）溶解于水中，加热至50~55℃，搅拌至溶液澄清透明；向体系中通入高纯氮气以除去溶解在水中的氧气，然后将反应体系升温至70℃~75℃，再向反应体系温中加入交联剂N，N-亚甲基双丙烯酰胺（MBA），搅拌8~15min，然后向反应体系中加入引发剂过硫酸铵（APS），搅拌聚合6~8h后冷却至室温，得到该剪切响应性水基凝胶润滑剂溶液。
丙烯酰胺（AM）和丙烯酸（AA）的摩尔比为3.5:1~4.5:1；丙烯酰胺（AM）和丙烯酸（AA）按1~1.5%的质量百分数溶于水中。
丙烯酰胺（AM）和N，N-亚甲基双丙烯酰胺（MBA）的摩尔比为40:1~65:1，N，N-亚甲基双丙烯酰胺（MBA）和过硫酸铵（APS）的摩尔比为1.5:1~1.8:1。
二、水基润滑剂的结构和性能
1、水基润滑剂的形貌
图1为本发明制备的水基凝胶润滑剂的外观图片。可见，本发明制备的水基润滑剂呈无色液态状，长期分散均匀稳定。初始的液态能使润滑剂更容易注入摩擦界面。
图2为本发明制备的水基凝胶润滑剂冷冻干燥后的扫描电子显微形貌。可见，冷冻干燥后的样品呈现出纤维状，这种结构能够使得在剪切过程中分子链呈剪切方向取向，赋予其剪切响应性。
图3为本发明制备的水基凝胶润滑剂的红外谱图。可见，AA和AM参与了聚合反应，得到了共聚物。
2、剪切响应特性
使用安东帕MCR 302流变仪研究了该水基凝胶润滑剂的剪切响应性，测试条件为：PP25平板测量***，狭缝宽度1mm，旋转模式，固定剪切频率，测量温度为25℃。
图4为本发明制备的水基凝胶润滑剂在0.5s-1的低剪切速率下的响应特性。由图4可知，水基凝胶润滑剂在0.5s-1的恒定剪切速率下，黏度随着剪切时间的延长而增大，剪切60s后变为凝胶状。剪切后水基凝胶润滑剂的宏观状态见图5，为凝胶状。
图6为水基凝胶润滑剂在100s-1剪切速率下响应特性。黏度曲线图6说明，本发明制备的水基凝胶润滑剂在高速剪切下仍然具有剪切增稠、成胶这一特殊性质。
3、摩擦学性能
采用HT-1000高温往复摩擦磨损试验机，具体实验条件为：载荷10N，不同频率，上试样为直径6mm的304不锈钢球或Si3N4陶瓷球。下试样分别为304不锈钢块和Si3N4陶瓷块。试验持续时间30min。
图7为在水润滑条件下的摩擦系数曲线，图7（a）是以不锈钢-不锈钢为摩擦副，平均摩擦系数约为0.32；其中图7（b）为以Si3N4-Si3N4为摩擦副，平均摩擦系数约为0.45。
图8为在本发明制备的水基润滑剂样品（实施例1）润滑条件下的摩擦系数曲线，以Si3N4-Si3N4为摩擦副，4Hz频率下平均摩擦系数约为0.188，与纯水润滑的Si3N4摩擦副相比，摩擦系数降低约60%。而且摩擦后的样品呈现出凝胶状吸附在摩擦副表面，证明了往复剪切也能够使该材料增稠、成胶。
图9为本发明制备的水基润滑剂润滑样品（实施例2）在不同频率下的摩擦系数曲线。以304-304不锈钢为摩擦副。具有快速频率响应特性。图9是以不锈钢-不锈钢为摩擦副，4Hz频率下平均摩擦系数低至0.262，与纯水润滑的304不锈钢摩擦副相比，摩擦系数降低约20%。摩擦后的样品也呈现出凝胶状吸附在摩擦副表面。
图8、9的结果表明，该水基凝胶润滑剂对不同的摩擦对偶具有响应特性，且随着往复频率的增大，摩擦系数逐渐减小，说明剪切频率越高，该水基润滑剂分子交联越快，越容易成胶。
综上所述，本发明剪切响应水基凝胶润滑剂基于高分子链的自组装构筑，有效解决了水润滑过程中膜形成能力不足、易发生粘着磨损的问题；所述水基凝胶润滑剂初始黏度较低，容易注入摩擦界面；具有快速剪切响应特性，在摩擦过程中迅速增稠，在摩擦界面上形成润滑膜，具有优异的粘附能力。用于摩擦配副时，不但能降低摩擦系数，而且能极大缓解摩擦界面的粘着磨损，这主要得益于剪切响应凝胶材料在摩擦界面上的成膜，避免了摩擦对偶的直接接触，从而实现了较好的摩擦学性能。另外，该剪切响应水基凝胶润滑剂在不同频率下有着不同的摩擦系数，因此有一定的工况适应性。并且对于不同的摩擦速度具有响应性。
附图说明
图1为本发明制备的水基凝胶润滑剂的宏观图片。
图2为本发明制备的水基凝胶润滑剂冷冻干燥后的扫描电子显微形貌。
图3为本发明制备的水基凝胶润滑剂胶红外图谱。
图4为本发明制备的水基凝胶润滑剂在0.5s-1剪切速率下的响应特性。
图5 为本发明制备的水基凝胶润滑剂剪切后的宏观状态。
图6为本发明制备的水基凝胶润滑剂在100s-1剪切速率下的响应特性。
图7为摩擦副在水润滑条件下的摩擦系数曲线。
图8为本发明制备的水基润滑剂润滑在不同频率下的摩擦系数曲线（Si3N4-Si3N4为摩擦副）。
图9为本发明制备的水基润滑剂润滑在不同频率下的摩擦系数曲线（304-304不锈钢为摩擦副）。
具体实施方式
下面通过具体实施例对本发明剪切响应性水基凝胶润滑剂的制备和应用性能作进一步说明。
实施例1
取23.10mmolAM、5.83mmolAA放入三口烧瓶中，加入130mL蒸馏水，在50℃下磁力搅拌至溶液澄清透明；向体系中通入高纯氮气20min以除去溶解在水中的氧气，然后将反应体系升温至70℃，再向体系中加0.52mmol的MBA，加热搅拌10min，加入0.26mmolAPS继续搅拌6h后冷却至室温，得到剪切响应性水基凝胶润滑剂。
以Si3N4-Si3N4作为摩擦副，在2Hz，4Hz，8Hz频率下测得水基凝胶润滑剂平均摩擦系数分别为0.271、0.188和0.146。
实施例2
取21.83mmolAM、5.28mmolAA放入三口烧瓶中，加入110ml蒸馏水，在50℃下磁力搅拌至溶液澄清透明；向体系中通入高纯氮气20 min以除去溶解在水中的氧气，然后将反体系升温至75℃，再向体系中加入0.38mmol的MBA，加热搅拌10min，加入0.17mmolAPS，加热搅拌7h后冷却至室温，得到该剪切响应性水基凝胶润滑剂。
以304-304不锈钢作为摩擦副，在2Hz，48Hz，8Hz频率下测得水基凝胶润滑剂的平均摩擦系数分别为0.287，0.262，0.231。

Claims (3)

1.一种剪切响应性水基凝胶润滑剂在润滑钢和氮化硅摩擦副中的应用，其特征在于：剪切响应水基凝胶润滑剂的制备方法为：将丙烯酰胺、丙烯酸溶解于水中，加热至50~55℃，搅拌至溶液澄清透明；向体系中通入高纯氮气以除去溶解在水中的氧气，然后将反应体系升温至70℃~75℃，再向反应体系中加入交联剂N,N-亚甲基双丙烯酰胺，搅拌8~15min，然后向反应体系中加入引发剂过硫酸铵，搅拌聚合6~8h后冷却至室温，得到该剪切响应性水基凝胶润滑剂溶液；丙烯酰胺和丙烯酸的摩尔比为3.5:1~4.5:1，丙烯酰胺和丙烯酸按1~1.5%的质量百分数溶于水中。
2.如权利要求1所述剪切响应性水基凝胶润滑剂在润滑钢和氮化硅摩擦副中的应用，其特征在于：丙烯酰胺和N,N-亚甲基双丙烯酰胺的摩尔比为40:1~65:1。
3.如权利要求1所述剪切响应性水基凝胶润滑剂在润滑钢和氮化硅摩擦副中的应用，其特征在于：N,N-亚甲基双丙烯酰胺和过硫酸铵的摩尔比为1.5:1~1.8:1。
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