石油学报(石油加工) ›› 2017, Vol. 33 ›› Issue (5): 849-857.doi: 10.3969/j.issn.1001-8719.2017.05.005

• 研究报告 • 上一篇    下一篇

纳米NiWO4硫化行为的实验研究

翟维明,李会峰,张乐,李明丰   

  1. 中国石化 石油化工科学研究院,北京 100083
  • 收稿日期:2016-11-07 修回日期:2017-03-14 出版日期:2017-09-25 发布日期:2017-11-29
  • 通讯作者: 李明丰, 男,教授级高级工程师,博士,从事加氢催化剂与工艺研究;Tel:010-82368628; E-mail:limf.ripp@sinopec.com E-mail:limf.ripp@sinopec.com
  • 作者简介:第一作者:翟维明,男,硕士,从事加氢催化剂研究
  • 基金资助:
    国家重点基础研究发展计划“973”项目(2012CB224802)资助

Experimental Study on the Sulfidation Behavior of NiWO4 Nanoparticles

ZHAI Weiming, LI Huifeng, ZHANG Le, LI Mingfeng   

  1. Research Institute of Petroleum Processing, SINOPEC, Beijing 100083, China
  • Received:2016-11-07 Revised:2017-03-14 Online:2017-09-25 Published:2017-11-29

摘要: 采用固相反应法和共沉淀法,通过改变水热处理温度和时间制备了一系列纳米NiWO4,考察了不同条件下制备的纳米NiWO4的硫化行为。分别采用X射线衍射(XRD)、扫描电镜(SEM)、程序升温硫化(TPS)、N2吸附-脱附(BET)、高分辨透射电镜(HRTEM)和X射线光电子能谱(XPS)等手段对硫化实验前后的样品进行了表征。结果表明,随着水热处理温度的升高或时间的延长,纳米NiWO4晶粒逐渐长大;TPS结果发现,在硫化过程中晶粒较小的纳米NiWO4仅在低温区间出现H2S吸收峰,晶粒较大的纳米NiWO4在低温区间和高温区间均出现H2S吸收峰,而晶粒尺寸增大后对扩散的影响是出现不同硫化行为的主要原因。

关键词: 纳米NiWO4, 水热处理;硫化行为;晶粒尺寸;程序升温硫化(TPS)

Abstract: A series of A series of NiWO4 nanoparticles were synthesized by the method of solidstate reaction and coprecipitation by imposing different temperatures and times of hydrothermal treatment. Sulfidation behaviors of NiWO4 nanoparticles prepared under different conditions were studied. The samples before and after sulfidation reaction were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), temperatureprogrammed sulfidation (TPS), N2 adsorptiondesorption(BET), high resolution transmission electron microscope (HRTEM) and Xray photoelectron spectroscopy (XPS), respectively. Results showed that with the increase of hydrothermal treatment temperature or time, the NiWO4 nanoparticle crystals gradually grew. TPS results showed that the H2S absorption peaks of the smaller NiWO4 nanoparticle crystals appeared only in the low temperature range during the TPS process. The H2S absorption peaks of the larger NiWO4 nanoparticle crystals appeared in both the low temperature range and the high temperature range. The effect of increased crystal size on diffusion was identified as the main reason for different sulfidation behaviors.

Key words: NiWO4 Nanoparticles, hydrothermal treatment, sulfidation behavior, crystal size, temperature-programmed sulfidation(TPS)