CN107916157B - 一种化学键结合的磷/碳复合物及其制备方法和应用 - Google Patents
一种化学键结合的磷/碳复合物及其制备方法和应用 Download PDFInfo
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Abstract
本发明公开了一种化学键结合的磷/碳复合物及其制备方法和应用,其特征在于所述复合物磷与碳通过磷‑氧‑碳共价键结合,原料组成包括红磷和碳,红磷和碳质量比为3:7~7:3。该复合物制备方法为:将不同质量比的红磷与碳材料分别在惰性气体保护下加入到球磨机中,密封后在高转速下球磨数十小时制得。该复合物作为高温润滑油减摩抗磨添加剂应用,可以在聚醚(PAG),聚乙二醇(PEG)等合成润滑油中形成稳定的分散体系,在温度50~200 oC范围内表现出优异的减摩抗磨性能。
Description
技术领域
本发明涉及一种化学键结合的磷/碳复合物及其制备方法,以及该复合物作为高温合成润滑油减摩抗磨添加剂的应用。
背景技术
许多不同类型的含磷化合物被作为润滑油添加剂来研究和应用,特别是作为潜在的减摩抗磨添加剂。例如中性三芳基磷酸酯、含金属的二硫代磷酸酯、含磷的离子液体。然而,传统方法制备含磷添加剂的过程冗长、污染大、成本高,这些缺点还有待进一步解决。
发明内容
本发明的目的在于提供一种新型高温润滑油固体添加剂—一种化学键结合的磷/碳复合物,该复合物通过球磨法制备,原料组成为红磷和碳,红磷和碳质量比为3:7~7:3,红磷与碳通过化学键结合,该化学键为磷-氧-碳共价键。
本发明的目的还在于提供一种球磨法制备化学键结合的磷/碳复合物的方法,具体为:
将不同质量比的红磷与碳材料(如石墨、石墨烯、碳纳米管等)分别在惰性气体保护下加入到球磨机中,密封后在高转速下球磨数十小时得到。
其中红磷与碳材料的质量比为3:7~7:3。所用惰性气体为氮气或氩气。在球磨机上研磨的时间为15~20 h,转速为200~400 rpm。
本发明的目的还在于提供上述化学键结合的磷/碳复合物作为高温润滑油减摩抗磨添加剂的应用。
本发明的优点在于:(1)通过球磨法制备的化学键结合的磷/碳复合物外观很松散,厚度很薄,这有利于增强其在润滑油中的分散稳定性。(2)上述化学键结合的磷/碳复合物可以在聚醚(PAG)、聚乙二醇(PEG)等合成酯类润滑油中形成稳定的分散体系,在高温环境下表现出优异的减摩抗磨性能。(3)本专利所述的球磨法生产过程简单,污染小。
附图说明
图1为红磷和实施例1,2,3中所述的红磷/石墨烯复合物(Gr-P)的高分辨扫描电子图像:a. 红磷,b. Gr-P( 7:3),c. Gr-P(1:1),d. Gr-P( 3:7);和石墨烯及相应Gr-P的透射电子显微图像:e. 石墨烯,f. Gr-P( 7:3),g. Gr-P(1:1),h. Gr-P(3:7)。
图2为聚醚(PAG),PAG中添加1.0% Gr(Gr为石墨烯),和PAG中添加0.1%,0.5%,1.0%,1.5%实施例3中制备的Gr-P,在100 oC,频率25 Hz,载荷100 N长磨30 min时的摩擦系数曲线。
图3为聚醚(PAG),PAG中添加1.0% Gr(Gr为石墨烯),和PAG中添加0.1%,0.5%,1.0%,1.5%实施例3中制备的Gr-P,在100 oC,频率25 Hz,载荷100 N长磨30 min时磨斑的磨损量。
图4为聚醚(PAG),PAG中添加1.0% Gr(Gr为石墨烯),和PAG中添加1.0%实施例3中制备的含Gr-P,在100 N,频率25 Hz,温度为25~200 oC时的摩擦系数曲线。
具体实施方式
将质量比为3:7~7:3的红磷和碳材料(如石墨、石墨烯、碳纳米管等)在惰性气体保护下加入球磨机中球磨15-20h,得到以化学键结合的磷/碳复合物,并将该复合物作为合成润滑油(如聚醚、聚乙二醇、酯类油)的添加剂,考察它们在高温下的减摩抗磨性能。
下面的实施例可以使本专业的技术人员更全面地理解本发明,但并不因此将本发明限制在所述的实施例范围之中。
实施例1
将 0.3g红磷和 0.7 g石墨烯在氮气保护下加入到碳化钨罐中,密封后在转速300rpm球磨16 h,待反应罐冷却后即可得到红磷/石墨烯复合物(Gr-P)。将得到的Gr-P按照浓度分别为0.1wt%,0.5wt%,1wt%和1.5wt%添加到聚醚(PAG)基础油中,机械搅拌30 min,之后再超声30 min。得到不同含量的Gr-P与PAG的分散体系。
实施例2
将0.5 g红磷和 0.5 g石墨烯在氮气保护下加入到碳化钨罐中,密封后在转速300rpm球磨16 h,待反应罐冷却后即可得到红磷/石墨烯复合物(Gr-P)。将得到的Gr-P按照浓度分别为0.1wt%,0.5wt%,1wt%和1.5wt%加入到聚醚(PAG)基础油中,机械搅拌30 min,之后再超声30 min。得到不同含量的Gr-P与PAG的分散体系。
实施例3
将 0.7g红磷和 0.3g石墨烯在氮气保护下加入到碳化钨罐中,密封后在转速300rpm球磨16 h,待反应罐冷却后即可得到红磷/石墨烯复合物(Cr-P)。将得到的Gr-P按照浓度分别为0.1wt%,0.5wt%,1wt%和1.5wt%加入到聚醚(PAG)基础油中,机械搅拌30 min,之后再超声30 min。得到不同含量的Gr-P与PAG的分散体系。
结构分析:将实施例1,2, 3的产物分散在无水乙醇中,通过JSM-6701F 冷场发射型扫描电镜和JEM-1200EX 透射电子显微镜测定其外观形貌,如附图1所示。结果表明,通过球磨法将红磷与石墨烯键合后形成的复合物外观很松散,厚度很薄,这有利于增强其在润滑油中的分散稳定性。
产物的摩擦学性能评价
1. 采用德国Optimol油脂公司生产的SRV-IV 微振动摩擦磨损试验机测试实施例3中制备的含0.1%,0.5%,1.0%,1.5% Gr-P的分散体系,在温度100 oC,频率25 Hz,振幅1mm,载荷100N,长磨30 min时的摩擦系数f,试验所用钢球为Φ=10 mm的GCr15轴承钢,下试样为Φ24×7.9 mm的GCr15钢块。结果见附图2。由图可以看出,在100℃,1.0% Gr-P可以显著降低PAG的摩擦系数。
2. 采用MicroXAM 3D 非接触的表面测试仪测试实施例3 中制备的含0.1%,0.5%,1.0%,1.5% Gr-P的分散体系,在温度100 oC,频率25 Hz,振幅1 mm,载荷100 N,长磨30 min时磨斑的磨损体积,如附图3所示。结果表明,在100℃, 0.5%,1.0% 和1.5% Gr-P均能显著增强PAG的抗磨性能。
3. 采用德国Optimol油脂公司生产的SRV-IV 微振动摩擦磨损试验机测试PAG,PAG中添加1.0% Gr(Gr为石墨烯),和PAG中添加1.0%实施例3中制备的Gr-P,在100 N,频率25 Hz,振幅1 mm,温度分别为25~200 oC时的摩擦系数曲线。结果表明,在升高温度时(>50 oC),Gr-P能够大幅度降低PAG的摩擦系数,并且Gr-P的减摩抗磨性能显著优于石墨烯。
以上显示和描述了本发明的基本原理和主要特征以及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (3)
1.一种化学键结合的磷/碳复合物作为高温润滑油减摩抗磨添加剂的应用,其特征在于:所述复合物中磷与碳通过化学键结合,该化学键为磷-碳共价键。
2.权利要求1所述化学键结合的磷/碳复合物作为高温润滑油减摩抗磨添加剂的应用,其特征在于,所述化学键结合的磷/碳复合物通过球磨法制备,原料组成包括红磷和碳,红磷和碳质量比为3:7~7:3。
3.权利要求1所述化学键结合的磷/碳复合物作为高温润滑油减摩抗磨添加剂的应用,其特征在于,所述化学键结合的磷/碳复合物制备方法具体如下:
将不同质量比的红磷与碳材料分别在惰性气体保护下加入到球磨机中,密封后在高转速下球磨数十小时,其中红磷与碳材料的质量比为3:7~7:3;
所用惰性气体为氮气或氩气;
所述高转速下球磨数十小时具体为转速200~400 rpm下球磨15~20 h。
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