无油硫磷酸的制备与研究

Preparation and Application of Oilless Sulfur Phosphate

以正丁醇、异辛醇、五硫化二磷为原料,在无溶剂的条件下,加入催化剂合成硫磷酸。考察催化剂种类、五硫化二磷加料方式、反应温度、真空度大小和初始加料温度对反应的影响。同时比较了此方法与老工艺合成的硫磷酸制备润滑油添加剂T202的性能差异。实验结果表明,此方法的最佳条件：选用催化剂4、五硫化二磷分9次加料、反应温度为50～55℃、真空度为0.07MPa、初始加料温度为40℃;在此条件下的反应时间为1h,硫磷酸收率可达99.4%;此条件合成的硫磷酸制备的润滑油添加剂T202的锌质量分数达11.76%,色度为0。

Sulfur phosphate was synthesized through the reaction of n-butanol, iso-octanol and phosphorus pentasulfide in the absence of solvent. The reaction condition was optimized by variation of catalyst type, the feeding mode of phosphorus pentasulfide, reaction temperature, pressure and initial reaction emperature. In the mean time, the performance differences of the lubricating additive T202 prepared by sulfur phosphate catalysis was compared with that synthesized with old process. Experimental results showed that the optimal conditions was as follows： the catalyst 4, the phosphorus pentasulfide feeding mode was nine, the reaction temperature was 50~55 ℃, the pressure was 0.07 MPa, initial temperature was 40 ℃, the reaction time was 1 h. Under this condition, the achieved content of sulfur phosphate was up to 99.4%, the zinc content of the lubricating additive T202 prepared by sulfur acid was 11.76%, and the chroma was 0.