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采用分子蒸馏技术对010型切割液进行分离,对分子蒸馏温度进行优化。当温度为80℃,刮板转速为300r/min,加料速率2mL/min,系统绝压20Pa时,分子蒸馏分离效果最佳。采用电喷雾质谱直接进样技术分析切割液各馏分,在正离子模式下,各组分可形成质子化分子或[M+NH4]+、[M+Na]+和[M+K]+等加合离子。以甲醇(1.0×10-3mol/L)-乙酸铵(90∶10 v/v)(流动相Ⅰ)为流动相时,[M+H]+、[M+NH4]+、[M+Na]+和[M+K]+4种PEG加合离子相对丰度均增加,[M+NH4]+峰增加尤为明显。对80℃分子蒸馏轻、重组分和PEG200进行电喷雾质谱表征时,以甲醇-水(90∶10 v/v)(流动相Ⅱ)为流动相,而对PEG400表征时则采用流动相Ⅰ。实验发现,采用流动相Ⅱ时轻组分与PEG200质谱分析结果类似,此时的重组分质谱结果与采用流动相Ⅰ时的PEG400类似。可推断,010#切割液主要成分为PEG200和PEG400,并含少量不挥发铵盐。
The molecular distillation technique was used to separate the 010 cutting fluid and optimize the molecular distillation temperature. When the temperature is 80 ℃, the speed of the scraper is 300r / min, the feeding rate is 2mL / min and the absolute pressure of the system is 20Pa, the molecular distillation separation effect is the best. The electrospray ionization mass spectrometry direct injection technique was used to analyze the fractions of the cutting fluid. In the positive ion mode, each molecule could form protonated molecules or [M + NH4] +, [M + Na] + and [M + K] + Addition of ions. [M + H] +, [M + NH4] +, [M + Na +] in the mobile phase of methanol (1.0 × 10-3 mol / L) ] + And [M + K] +4 kinds of PEG adducts increased, especially the increase of [M + NH4] +. When methanol, water (90:10 v / v) (mobile phase II) was used as the mobile phase for the characterization of PEG400, the mobile phase Ⅰ was used to characterize PEG400. The experimental results showed that the light fraction of mobile phase Ⅱ was similar to that of PEG200. The results of mass spectrometry were similar to that of PEG400 using mobile phase Ⅰ. It can be inferred that 010 # cutting fluid main components PEG200 and PEG400, and contains a small amount of non-volatile ammonium salt.