CN113913229A - 一种基于黑水虻油脂的环境友好型抗磨添加剂及其制备方法 - Google Patents
一种基于黑水虻油脂的环境友好型抗磨添加剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种基于黑水虻油脂的环境友好型抗磨添加剂及其制备方法,所述抗磨添加剂由黑水虻油脂经转酯化反应、硫化反应得到。本发明提供的基于黑水虻油脂的环境友好型抗磨添加剂具有优异的高温抗氧化性、低温流动性以及生物可降解性,其在100℃下的运动黏度为64.5~66.7mm2/s,倾点为‑15℃,最大无卡咬负荷PB值为1254N,烧结负荷PD值为3087N,旋转氧弹时间为35~38min。
Description
技术领域
本发明属于以反应产物为特征的润滑组合物,具体涉及一种基于黑水虻油脂的环境友好型抗磨添加剂及其制备方法。
背景技术
近年来,我国金属加工液市场需求持续增长。金属加工液根据用途不同可分为金属成型液、金属切削液、金属防护液和金属处理液四大类,其中抗磨剂是金属加工液中的主要成份,其作用为在金属接触表面形成保护膜降低摩擦磨损。
抗磨剂分子结构中含有硫、磷、氯等活性元素,可以与金属表面发生化学反应形成保护膜来实现对摩擦副的保护作用。其中含硫抗磨剂主要包括硫化动植物油、硫化烃、硫代酯、多硫化物等。国内外以前大量使用硫化鲸鱼油作为油性剂,鲸鱼油经过一系列化学改性而制成各种工业用途的润滑剂和极压剂、油性剂,具有优异的润滑性能,曾被广泛地用于自动传动液、金属加工液、工业齿轮油和各种液压油等油品中。《全球禁止捕鲸公约》通过后,各国大力发展硫化鲸鱼油的代替品,国内外先后研制了硫化烯烃、硫化棉籽油、硫化酯等产品。
CN1176068C、CN103923062A等专利公开报告了硫化异丁烯以及衍生物的制备方法,这类含有活性硫的抗磨添加剂具有超过40%的硫含量以及优异的抗磨性能,目前广泛应用于齿轮油的配方体系中。然而,硫化异丁烯具有强烈的气味且生产过程中会产生大量废水,不符合新一代环保型抗磨剂的发展要求。基于植物油直接硫化得到的硫化棉籽油、硫化酯等含硫抗磨剂虽然具有良好的生物降解性,但是,较差的高温抗氧性导致产生严重的油泥和积碳,较差的低温流动性导致产品无法快速到达摩擦副表面实现润滑作用,这些劣势限制了这类产品的应用。相对于植物而言,昆虫具有较短的生长周期,繁殖迅速,生物量大,饲养成本低的优点,具有非常良好的资源化利用前景,但目前基于昆虫油脂的抗磨材料应用研究较少。
发明内容
本发明所要解决的技术问题是针对现有技术中存在的上述不足,提供一种基于黑水虻油脂的环境友好型抗磨添加剂及其制备方法,该抗磨剂具有优异的高温抗氧化性、低温流动性以及生物可降解性。
为解决上述技术问题,本发明提供的技术方案是:
提供一种基于黑水虻油脂的环境友好型抗磨添加剂,所述抗磨添加剂由黑水虻油脂经转酯化反应、硫化反应得到。
按上述方案,所述环境友好型抗磨添加剂在100℃下的运动黏度为64.5~66.7mm2/s,倾点为-15℃,最大无卡咬负荷PB值为1254N,烧结负荷PD值为3087N,旋转氧弹时间为35~38min。
按上述方案,所述黑水虻油脂为7-10日龄黑水虻幼虫中提取的油脂。黑水虻幼虫经干燥、萃取、脱酸、脱色工艺即可得到黑水虻油脂,提取工艺参见:J Am OilChem Soc(2020)97:1243–1251。
本发明还包括上述基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,具体步骤如下:
1)以黑水虻油脂和短链醇为原料,在硫酸作为催化剂的条件下进行转酯化反应,反应结束后静置至反应液分层,收集上层油状产物;
2)向步骤1)所得油状产物中加入催化剂,在氮气保护下加入升华硫进行硫化反应,反应结束后冷却至50~55℃进行抽滤,除去固体杂质后得到深色粘稠液体,即基于黑水虻油脂的环境友好型抗磨添加剂。
按上述方案,步骤1)所述短链醇为甲醇,乙醇,丙醇,异丙醇,丁醇中的一种,所述黑水虻油脂和短链醇的摩尔比为1:1.1~1.2。
按上述方案,步骤1)所述转酯化反应条件为:70~90℃反应8~9小时。
按上述方案,步骤2)所述催化剂为磷酸钙,催化剂的质量为油状产物质量的1~1.2%。
按上述方案,步骤2)所述升华硫的质量为油状产物质量的9~11%。优选为10%。
按上述方案,步骤2)所述硫化反应条件为:在惰性气氛下,于140~160℃反应6~8小时。
本申请所提供的环境友好型抗磨添加剂含硫,其与金属如铁表面接触在摩擦过程中产生的高温和高压环境下抗磨剂与金属表面反应生成含硫的无机膜(Fe2O3-FeS的极压化学反应膜),从而起到抗擦伤和抗烧结的作用。
本发明的有益效果在于:1、本发明提供的基于黑水虻油脂的环境友好型抗磨添加剂具有优异的高温抗氧化性、低温流动性以及生物可降解性,其在100℃下的运动黏度为64.5~66.7mm2/s,倾点为-15℃,最大无卡咬负荷PB值为1254N,烧结负荷PD值为3087N,旋转氧弹时间为35~38min。2、本发明的制备方法以黑水虻油脂为原料,原料生产周期短,工艺简单,条件温和,产生的废弃物少,成本低,适合大规模生产。
附图说明
图1为本发明实施例1制备的基于黑水虻油脂的环境友好型抗磨添加剂与对比例1硫化烯烃棉籽油T405随着负载增加摩擦系数变化曲线图;
图2为实施例1制备的基于黑水虻油脂的环境友好型抗磨添加剂的红外光谱图;
图3为实施例1抗磨添加剂进行四球长时间磨损后磨斑表面EDAX能谱图。
具体实施方式
为使本领域技术人员更好地理解本发明的技术方案,下面结合附图对本发明作进一步详细描述。
本发明实施例所用黑水虻油由武汉工程大学提供,提取工艺参见J Am OilChemSoc(2020)97:1243–1251。
实施例1
一种基于黑水虻油脂的环境友好型抗磨添加剂,其制备方法步骤如下:
1)按质量份计,称取100份黑水虻油、33.5份无水乙醇和0.5份浓硫酸(98wt%)加入到烧瓶中,加热到80℃,机械搅拌反应8小时后静置至室温,反应液分层,收集上层油状产物;
2)按质量份计,称取步骤1)所得油状产物100份,10份升华硫以及1份磷酸钙加入到三口烧瓶中,在氮气保护下升温至150℃反应6小时,反应过程中保持搅拌状态使各组分充分混合,反应结束后冷却至50℃进行抽滤,除去固体杂质后得到深色粘稠液体即为目标产品。
本实施例所得产物为深色粘稠状液体,不溶于水,闪点在180℃左右,产物在空气中加热至150℃保温72h,质量和状态无明显变化,化学性质稳定。
本实施例制备的抗磨添加剂的红外光谱图如图2所示,其中1741cm-1处为C=O的伸缩振动吸收峰,1236cm-1和1164cm-1处为C-O伸缩振动吸收峰,973cm-1处的吸收峰为链状C-S的特征吸收峰,确认了硫化反应的进行。
采用《GB/T 3142-2019润滑剂承载能力的测定四球法》测试本实施例制备的抗磨添加剂,使用EDAX能谱对四球长时间磨损后磨斑表面进行表面元素分析(EDAX条件:激发源功率为200W,分析时的基础真空度5×10-10mbar),所得膜层表面元素对比图见图3,膜层中检测到C、N、O、Fe、S、Si、Cr、Fe等元素的存在,其中Si、Fe和Cr来自钢球本身,S和O元素来自于润滑油,推测在摩擦过程中产生的高温和高压环境下抗磨剂与金属表面反应生成含硫的无机膜,形成0.15微米以上的Fe2O3-FeS的极压化学反应膜,从而起到抗擦伤和抗烧结的作用。
对比例1
硫化烯烃棉籽油T405,沧州市亿达渤润石化有限公司生产。
实施例1制备的基于黑水虻油脂的环境友好型抗磨添加剂以及对比例1的硫化烯烃棉籽油T405的性能测试结果如表1所示:
表1
项目 | 实施例1 | 对比例1 | 试验方法 |
运动黏度(100℃)/(mm<sup>2</sup>/s) | 64.5 | 80.9 | GB/T 265-1988 |
外观 | 棕色透明 | 棕色透明 | 目测 |
倾点/℃ | -15 | -9 | GB/T 3535-2006 |
最大无卡咬负荷P<sub>B</sub>/N<sup>1</sup> | 1254 | 1117 | GB/T 3142-2019 |
烧结负荷P<sub>D</sub>/N<sup>2</sup> | 3087 | 3087 | GB/T 3142-2019 |
旋转氧弹/min | 38 | 27 | SH/T 0193-2008 |
闪点/℃ | 170 | 156 | GB/T 3536-2008 |
注:1、2均为相应样品溶于惠州150N基础油中(质量浓度5%)检测
由表1可知,本申请实施例制备的基于黑水虻油脂的环境友好型抗磨添加剂与硫化烯烃棉籽油T405相比,100℃下运动黏度低,倾点低,最大无卡咬负荷PB值高,旋转氧弹时间长,说明其抗擦伤和高温抗氧化性能更优异。
如图1所示为本申请实施例1制备的基于黑水虻油脂的环境友好型抗磨添加剂与对比例1硫化烯烃棉籽油T405随着负载增加,摩擦系数变化曲线(测试条件:初始载荷为50N,逐步增加至最大1600N,实验温度50℃,行程1.0mm),可以看出,随着负载的增加,实施例1制备的环境友好型抗磨添加剂与对比例1硫化烯烃棉籽油T405的摩擦系数下降15%左右,具有明显优异的抗磨性能。
Claims (9)
1.一种基于黑水虻油脂的环境友好型抗磨添加剂,其特征在于,所述抗磨添加剂由黑水虻油脂经转酯化反应、硫化反应得到。
2.根据权利要求1所述的基于黑水虻油脂的环境友好型抗磨添加剂,其特征在于,所述环境友好型抗磨添加剂在100℃下的运动黏度为64.5~66.7mm2/s,倾点为-15℃,最大无卡咬负荷PB值为1254N,烧结负荷PD值为3087N,旋转氧弹时间为35~38min。
3.根据权利要求1所述的基于黑水虻油脂的环境友好型抗磨添加剂,其特征在于,所述黑水虻油脂为7-10日龄黑水虻幼虫中提取的油脂。
4.一种权利要求1-3任一所述的基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,其特征在于,具体步骤如下:
1)以黑水虻油脂和短链醇为原料,在硫酸作为催化剂的条件下进行转酯化反应,反应结束后静置至反应液分层,收集上层油状产物;
2)向步骤1)所得油状产物中加入催化剂,在氮气保护下加入升华硫进行硫化反应,反应结束后冷却至50~55℃进行抽滤,除去固体杂质后得到深色粘稠液体,即基于黑水虻油脂的环境友好型抗磨添加剂。
5.根据权利要求4所述的基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,其特征在于,步骤1)所述短链醇为甲醇,乙醇,丙醇,异丙醇,丁醇中的一种,所述黑水虻油脂和短链醇的摩尔比为1:1.1~1.2。
6.根据权利要求4所述的基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,其特征在于,步骤1)所述转酯化反应条件为:70~90℃反应8~9小时。
7.根据权利要求4所述的基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,其特征在于,步骤2)所述催化剂为磷酸钙,催化剂的质量为油状产物质量的1~1.2%。
8.根据权利要求4所述的基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,其特征在于,步骤2)所述升华硫的质量为油状产物质量的9~11%。
9.根据权利要求4所述的基于黑水虻油脂的环境友好型抗磨添加剂的制备方法,其特征在于,步骤2)所述硫化反应条件为:在惰性气氛下,于140~160℃反应6~8小时。
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