石油炼制与化工 ›› 2022, Vol. 53 ›› Issue (11): 123-127.

• 分析与评定 • 上一篇    下一篇

浆态床渣油加氢物料中钼含量的测定方法研究

侯小敏,王轲,徐茜,吴梅   

  1. 中石化石油化工科学研究院有限公司
  • 收稿日期:2022-03-15 修回日期:2022-05-24 出版日期:2022-11-12 发布日期:2022-11-02
  • 通讯作者: 吴梅 E-mail:wumei.ripp@sinopec.com

DETERMINATION METHOD OF MOLYBDENUM CONTENT IN SLURRY BED RESIDUE HYDROCRACKING MATERIALS


  • Received:2022-03-15 Revised:2022-05-24 Online:2022-11-12 Published:2022-11-02
  • Contact: Wu Mei E-mail:wumei.ripp@sinopec.com

摘要: 采用干灰化的样品预处理方法,使用电感耦合等离子体发射光谱仪,建立浆态床渣油加氢物料中钼(有机钼和无机钼)含量测定的分析方法。考察样品前处理过程中的灰化温度、灰化时间和酸处理条件等对钼含量测定的影响。结果表明,当灰化温度为430~480 ℃、灰化时间不小于10 h、溶解灰分的酸为盐酸或硝酸时,可准确测定浆态床渣油加氢物料中的钼(有机钼和无机钼)含量。该方法的相对标准偏差不大于1%,加标回收率为97%~102%。满足元素分析的一般要求。与国家标准GB/T 37160—2019方法相比,该方法降低了灰化温度,减少了酸用量,钼含量测定结果更准确。

关键词: 浆态床, 渣油加氢, 干灰化, 钼含量

Abstract: A method for the determination of molybdenum (organic molybdenum and inorganic molybdenum) in slurry bed residue hydrocrackting materials was established by using a dry ashing pretreatment method and an inductively coupled plasma optical emission spectrometry. The effects of ashing time, ashing temperature and acid treatment on the determination of molybdenum element were investigated. The results showed that the content of molybdenum (organic molybdenum and inorganic molybdenum) could be accurately determined when the ashing temperature was 430-480 ℃, ashing time was not less than 10 h, the acid dissolving the ash was hydrochloric acid or nitric acid. The relative standard deviation of this method was less than 1%, and the recovery was 97%-102%, met the general requirements of elemental analysis. Compared with GB/T 37160—2019, this method can reduce the ashing temperature, reduce the amount of acid, and determine the molybdenum content more accurately.

Key words: slurry bed, residue hydrotreating, dry ashing, molybdenum content