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作 者:曹毅[1] 马楷[1] CAO Yi;MA Kai(Synthetic Lubricants Branch of Sinopec Lubricant Co.,Ltd.,Chongqing 400039,China)
机构地区:[1]中国石化润滑油有限公司合成油脂分公司,重庆400039
出 处:《石油化工》2024年第5期655-661,共7页Petrochemical Technology
摘 要:以季戊四醇与亚磷酸、脂肪酸为原料,采用两步法合成工艺制备了含磷季戊四醇酯,利用FTIR、NMR及元素分析对其结构进行表征,并对其高温稳定性进行评价。实验结果表明,第一步酯化反应在170~185℃下,无催化剂的体系反应效果与硫酸催化反应体系接近且优于氧化亚锡体系,说明亚磷酸在反应体系中既作底物,同时又起到了催化作用;第二步酯化反应在220~230℃下,无催化剂的亚磷酸体系与表现最佳催化效果的氧化亚锡体系的反应效果相当,进一步说明亚磷酸具有良好的自催化能力。与未进行亚磷酸改性的季戊四醇酯(典型的MIL-PRF-23699规范基础油)相比,含磷季戊四醇酯润滑油的分解温度提升约76℃,HPDSC氧化温度提升约25℃,表明亚磷酸改性可很好地提升季戊四醇酯润滑油的高温性能,使其在高温领域的应用得到拓展。Phosphorous pentaerythritol esters were prepared by a two-step synthesis process,with pentaerythritol,phosphorous acid,and fatty acids used as raw materials.Their structures were characterized by FTIR,NMR,and elemental analysis,and their high-temperature stability was further evaluated.The experimental results show that the first step of the esterification reaction proceeds at 170-185℃,and the reaction effect of the system without a catalyst is accessible to that of the sulfuric acid catalytic reaction system and superior to that of the stannous oxide system,indicating that phosphorous acid not only acts as a substrate but also plays a catalytic role in the reaction system.The second step of the esterification reaction proceeds at 220-230℃,and the reaction effect achieved by the phosphorous acid system without a catalyst is comparable to that of the stannous oxide system with the best catalytic performance,further indicating that phosphorous acid possesses an excellent autocatalysis ability.Compared with unmodified pentaerythritol ester by phosphorous acid(typical MIL-PRF-23699 standard base oil),the decomposition temperature of the lubricating oil containing phosphorus pentaerythritol ester has increased by about 76℃,and the oxidation temperature detected by HPDSC has increased by about 25℃.This indicates that phosphorous acid modification can effectively improve the high-temperature performance of lubricating oil containing pentaerythritol esters,expanding its application in the high-temperature field.
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