石油炼制与化工 ›› 2023, Vol. 54 ›› Issue (5): 113-119.

• 分析与评定 • 上一篇    下一篇

炼油废催化剂中石油烃的提取和分析

马苏甜,万伟,钱钦,韩旭,刘颖荣   

  1. 中石化石油化工科学研究院有限公司
  • 收稿日期:2022-09-05 修回日期:2022-12-21 出版日期:2023-05-12 发布日期:2023-05-12
  • 通讯作者: 马苏甜 E-mail:masutian.ripp@sinopec.com

EXTRACTION AND ANALYSIS OF PETROLEUM HYDROCARBONS FROM REFINERY WASTE CATALYSTS

  • Received:2022-09-05 Revised:2022-12-21 Online:2023-05-12 Published:2023-05-12

摘要: 采用加速溶剂萃取-气相色谱法,建立了炼油废催化剂中C10~C40石油烃的提取和分析方法,考察了不同填料的固相萃取柱及洗脱溶剂的净化效果,并对气相色谱分析条件进行了优化,评价了该方法的准确度及回收率。结果表明:适合石油烃净化的萃取柱为硅酸镁柱或硅胶固相萃取柱,适宜的洗脱溶剂分别为体积比4:1的正己烷/二氯甲烷混合溶剂(硅酸镁柱)和体积比9:1的正己烷/二氯甲烷混合溶剂(硅胶柱);两种萃取柱的多环芳烃回收率均为94%~100%;在优化的气相色谱条件下,正构烷烃校准曲线的线性相关系数为0.999 3,相对偏差为0.6%~10.9%,正构烷烃和重油的回收率分别为74%和84%,说明所建方法可以满足炼油废催化剂中石油烃的监测要求。利用该方法对废催化剂样品进行处理,发现不同来源的炼油废催化剂中石油烃(C10~C40)的碳数分布和含量均存在显著差异,这主要与废催化剂对应的工艺及原料有关。

关键词: 炼油厂, 废催化剂, 石油烃, 提取, 净化, 气相色谱

Abstract: A method for the extraction and analysis of C10-C40 petroleum hydrocarbons in refinery waste catalysts was established by using accelerated solvent extraction-gas chromatography method. The purification effects of solid phase extraction columns with different packings and elution solvents were investigated. The analysis conditions of gas chromatography were optimized, and the accuracy and the recovery rate of the method were evaluated. The results showed that the suitable column for petroleum hydrocarbon extraction was magnesium silicate column or silica gel solid phase extraction column, and the suitable elution solvents were n-hexane-dichloromethane mixed solvent with a volume ratio of 4:1(magnesium silicate column) and n-hexane-dichloromethane mixed solvent with a volume ratio of 9:1(silica gel column) , respectively. The polycyclic aromatic hydrocarbon recoveries of the two extraction columns were 94%-100%, and the calibration curves of n-alkanes were determined by GC-FID with a relative deviation of 0.6%-10.9% and a 0.999 3, respectively; the recoveries of n-alkanes and heavy oil were 74% and 84%, respectively, which showed that the method could meet the analysis of petroleum hydrocarbons in refinery waste catalysts. The carbon number distribution and content of petroleum hydrocarbon (C10-C40) in different sources of refinery catalyst were found to be significantly different, this was mainly related to the corresponding process and raw material characteristics of the waste catalyst.

Key words: refinery, waste catalyst, petroleum hydrocarbons, extraction, purify, gas chromatography