CN113046164B - 一种环境响应型水基润滑剂及其制备方法 - Google Patents
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Abstract
本案涉及一种环境响应型水基润滑剂及其制备方法,是由0.5~1wt%的微凝胶添加剂、0.6~1.5wt%的壳聚糖添加剂和水组成;其中所述微凝胶添加剂由温敏性聚合物与两性化合物首先通过聚合反应制得共聚物,再与功能化石墨烯反应得到的一种含石墨烯的温敏微凝胶。本发明的环境响应型水基润滑剂具有较低的摩擦系数,常规条件下可将纯水的摩擦系数降低至0.15左右;且对温度和pH值敏感,当温度超过LCST值或pH低于6.0时,水基润滑剂会显示出较大的润滑性能,摩擦系数进一步可降低至0.1左右。
Description
技术领域
本发明属于水基润滑剂技术领域,具体为一种环境响应型水基润滑剂及其制备方法。
背景技术
在工业生产中,大多使用由矿物油炼制成的油类润滑剂或润滑脂来提高机械系统的减摩抗摩性能,以延长机械系统的使用寿命,但该类润滑剂存在成本高,对环境会造成污染等问题。且随着人类环保意识的加深,人们越来越倡导绿色可持续发展,因此尝试用水来代替由矿物油炼制成的油类润滑剂成为近年来的研究重点。
然而由于水的粘度低,水基润滑剂存在成模性较差的问题,很难在润滑界面形成稳定的具有抗摩减摩作用的润滑膜,限制了其在实际中的应用。而油基添加剂的使用能够很好的提高水的润滑性能。目前,针对这方面的研究很多,但鲜少有将环境响应型材料与之结合的案例,环境响应材料与传统材料相比最大的优点在于其能对外场刺激发生可逆且可控的性能变化。在某些应用场景下,当环境改变时需要水基润滑剂产生更大的润滑性能,当环境不曾改变时,充当普通润滑剂,这样可以增加水基润滑剂的使用寿命。
发明内容
针对现有技术中的不足之处,本发明旨在提供一种对环境如温度和pH具有响应性的水基润滑剂以填补目前水基润滑剂种类中智能材料的空缺。
为实现上述目的,本发明提供如下技术方案:
一种环境响应型水基润滑剂的制备方法,包括以下步骤:
一、制备微凝胶添加剂
1)将温敏性聚合物和两性化合物加入到反应装置中,向瓶中通入氮气,随后加入N,N'-亚甲基双丙烯酰胺、溴化亚铜和N,N,N',N”,N”'-五甲基二亚乙基三胺,加水和表面活性剂搅拌使其混合均匀,随后滴加2-溴丙酸乙酯,在氮气氛围下密封反应4-6h,得到乳白色微凝胶溶液;
2)向步骤1)中添加石墨烯和催化量的二氮杂二环,40~50℃下反应3-5h,得到含石墨烯的温敏微凝胶;
3)使用去离子水透析制得的含石墨烯的温敏微凝胶,经过5-7天透析处理即制得所述添加剂;
二、制备壳聚糖添加剂
配置壳聚糖的浓度为20-30mg/ml,加氢氧化钠调节pH至6±0.2,将壳聚糖水溶液装入透析袋中,用pH为7.4的磷酸缓冲液透析5天,制得壳聚糖添加剂;
三、将所述微凝胶添加剂和壳聚糖添加剂混合后加水稀释制得响应型水基润滑剂。
进一步地,所述温敏性聚合物为聚乙二醇丙烯酸甲酯或聚丙烯酸乙氧基乙氧基乙酯,所述两性化合物为[2-(甲基丙烯酰基氧基)乙基]二甲基-(3-磺酸丙基)氢氧化铵,所述功能化石墨烯为羧基化石墨烯。
进一步地,所述温敏性聚合物、两性化合物、交联单体、催化剂、配体和引发剂的摩尔比为50:10~50:1.5:1:2:1。
进一步地,各组分的质量分数为0.5~1wt%的微凝胶添加剂、0.6~1.5wt%的壳聚糖添加剂和水组成。
本发明提供一种采用如上所述的制备方法制得的环境响应型水基润滑剂。
本发明的有益效果是:本发明的环境响应型水基润滑剂具有较低的摩擦系数,常规条件下可将纯水的摩擦系数降低至0.15左右;且对温度和pH值敏感,当温度超过LCST(临界胶束浓度)值或pH低于6.0时,水基润滑剂会显示出较大的润滑性能,摩擦系数进一步可降低至0.11左右。
附图说明
图1为本案实施例中各水基润滑剂的摩擦系数随温度变化的关系图。
具体实施方式
下面将结合实施例对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
此外,下面所描述的本发明不同实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互结合。
PEGA(Mn=480g/mol)、PEGMA(Mn=500g/mol)、MSA纯度大于98%,购于ALDRICH,过中性氧化铝低温保存;2-溴丙酸乙酯、2-溴异丁酸乙酯、2-溴丙烯酸乙酯、壳聚糖购于百灵威(上海)科技有限公司,直接使用;DBU日本东京化成工业株式会社;BIS购于上海笛柏生物科技有限公司;SDBS、SDS和NP-10购于上海伊卡生物技术有限公司;PMDETA购于上海吉至生化科技有限公司;溴化亚铜、溴化铜购于安耐吉化学,直接使用;羧基化石墨烯粉末,0.5-5μm厚,购自先丰纳米。
实施例1:一种环境响应型水基润滑剂
1)将10mmol PEGA和2mmol MSA加入到反应装置中,向瓶中通入氮气,随后加入0.3mmol BIS、0.2mmol溴化亚铜和0.4mmol PMDETA,加1gSDBS以及200ml水搅拌使其混合均匀,随后滴加0.2mmol 2-溴丙酸乙酯,在氮气氛围下密封反应4-6h,得到乳白色微凝胶溶液;
2)向步骤1)中添加1g羧基化石墨烯粉末和催化量的DBU,40~50℃下反应3-5h,得到含石墨烯的温敏微凝胶;
3)使用去离子水透析制得的含石墨烯的温敏微凝胶,经过5-7天透析处理即制得微凝胶添加剂;
配置壳聚糖的浓度为20mg/ml,加氢氧化钠调节pH至6±0.2,将壳聚糖水溶液装入透析袋中,用pH为7.4的磷酸缓冲液透析5天,制得壳聚糖添加剂。
将所述微凝胶添加剂和壳聚糖添加剂混合后加水稀释,使微凝胶的含量达到0.8wt%,壳聚糖的含量达到1.0wt%,制得响应型水基润滑剂。
实施例2:一种环境响应型水基润滑剂
1)将10mmol PEGA和6mmol MSA加入到反应装置中,向瓶中通入氮气,随后加入0.3mmol BIS、0.2mmol溴化铜和0.4mmol PMDETA,加1gNP-10以及200ml水搅拌使其混合均匀,随后滴加0.2mmol 2-溴丙酸乙酯,在氮气氛围下密封反应4-6h,得到乳白色微凝胶溶液;
2)向步骤1)中添加1g羧基化石墨烯粉末和催化量的DBU,40~50℃下反应3-5h,得到含石墨烯的温敏微凝胶;
3)使用去离子水透析制得的含石墨烯的温敏微凝胶,经过5-7天透析处理即制得微凝胶添加剂;
配置壳聚糖的浓度为20mg/ml,加氢氧化钠调节pH至6±0.2,将壳聚糖水溶液装入透析袋中,用pH为7.4的磷酸缓冲液透析5天,制得壳聚糖添加剂。
将所述微凝胶添加剂和壳聚糖添加剂混合后加水稀释,使微凝胶的含量达到1wt%,壳聚糖的含量达到1.2wt%,制得响应型水基润滑剂。
实施例3:一种环境响应型水基润滑剂
1)将10mmol PEGA和10mmol MSA加入到反应装置中,向瓶中通入氮气,随后加入0.3mmol BIS、0.2mmol溴化亚铜和0.4mmol PMDETA,加1g SDS以及200ml水搅拌使其混合均匀,随后滴加0.2mmol 2-溴异丁酸乙酯,在氮气氛围下密封反应4-6h,得到乳白色微凝胶溶液;
2)向步骤1)中添加1g羧基化石墨烯粉末和催化量的DBU,40~50℃下反应3-5h,得到含石墨烯的温敏微凝胶;
3)使用去离子水透析制得的含石墨烯的温敏微凝胶,经过5-7天透析处即制得微凝胶添加剂;
配置壳聚糖的浓度为20mg/ml,加氢氧化钠调节pH至6±0.2,将壳聚糖水溶液装入透析袋中,用pH为7.4的磷酸缓冲液透析5天,制得壳聚糖添加剂。
将所述微凝胶添加剂和壳聚糖添加剂混合后加水稀释,使微凝胶的含量达到1wt%,壳聚糖的含量达到1.5wt%,制得响应型水基润滑剂。
实施例1-3的LCST值记录在表1中,测试水基润滑剂的摩擦摩擦性能,测试条件为钢-钢摩擦副、接触形式为球盘点接触,运动方式为往复运动型,载荷设置为50N,频率为15Hz,滑动时间30min,测试该水基润滑剂在常规条件下(室温、中性环境)的润滑性能,以及其温度和pH的响应性。结果记录在表1中。
表1
如表1所示,常规条件下水基润滑剂的摩擦系数仅有0.16左右,当温度升高或pH减小时,其表现出更低的润滑性能。
纯水在温度升高的过程中摩擦系数会有所上升,部分微凝胶在温度升至LCST值时也会有升高的倾向,温度超过LCST时,摩擦系数才会逐渐降低。本案将温度范围设置为各水基润滑剂LCST的正负5℃范围内,纯水温度设置为25-35-45-55-65℃;此外,以常规温敏性微凝胶制备水基润滑剂,将PNIPAM配制成1wt%水溶液作润滑剂,LCST为37℃,同样设置温度为LCST的正负5℃范围内。如图1所示,纯水的摩擦系数则逐渐变大,其摩擦系数从0.45上升至0.5左右;含1wt%PNIPAM的润滑剂的摩擦系数在温度升高过程中先升高再减小;而本发明的水基润滑剂在温度升高的变化过程中摩擦系数逐渐减小,各摩擦系数随着温度的升高逐渐减小至0.10左右。
本发明的水基润滑剂可以实现根据外界环境变化自我调节的功能,弥补了智能水基润滑剂的空缺。
尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节。
Claims (4)
1.一种环境响应型水基润滑剂的制备方法,其特征在于,包括以下步骤:
一、制备微凝胶添加剂
1)将温敏性聚合物和两性化合物加入到反应装置中,向瓶中通入氮气,随后加入交联单体N,N'-亚甲基双丙烯酰胺、催化剂溴化亚铜和配体N,N,N',N'',N'''-五甲基二亚乙基三胺,加水和表面活性剂搅拌使其混合均匀,随后滴加引发剂2-溴丙酸乙酯,在氮气氛围下密封反应4-6h,得到乳白色微凝胶溶液;
2)向步骤1)中添加石墨烯和催化量的二氮杂二环,40~50℃下反应3-5h,得到含石墨烯的温敏微凝胶;
3)使用去离子水透析制得的含石墨烯的温敏微凝胶,经过5-7天透析处理即制得所述添加剂;
二、制备壳聚糖添加剂
配置壳聚糖的浓度为20-30mg/ml,加氢氧化钠调节pH至6±0.2,将壳聚糖水溶液装入透析袋中,用pH为7.4的磷酸缓冲液透析5天,制得壳聚糖添加剂;
三、将所述微凝胶添加剂和壳聚糖添加剂混合后加水稀释制得响应型水基润滑剂;其中,
所述温敏性聚合物为聚乙二醇丙烯酸甲酯或聚丙烯酸乙氧基乙氧基乙酯,所述两性化合物为[2-(甲基丙烯酰基氧基)乙基]二甲基-(3-磺酸丙基)氢氧化铵,所述石墨烯为羧基化石墨烯。
2.如权利要求1所述的环境响应型水基润滑剂的制备方法,其特征在于,所述温敏性聚合物、两性化合物、交联单体、催化剂、配体和引发剂的摩尔比为50:10~50:1.5:1:2:1。
3.如权利要求1所述的环境响应型水基润滑剂的制备方法,其特征在于,水基润滑剂由质量分数为0.5~1wt%的微凝胶添加剂、0.6~1.5wt%的壳聚糖添加剂和水组成。
4.一种采用如权利要求1-3中任一项所述的制备方法制得的环境响应型水基润滑剂。
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