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Preparation and hydrodesulfurization performance of Al-MCM-41-supported nickel phosphide catalysts

KUANG Zhimin1,GONG Jianyi2,YANG Yunquan1,WANG Weiyan1,CHEN Laifu1,HE Heng1   

  1. (1School of Chemical Engineering,Xiangtan University,Xiangtan 411105,Hunan,China;2 Catalyst Company,SINOPEC,Beijing 100011,China)
  • Online:2011-03-05 Published:2011-03-05

Ni2P/Al-MCM-41催化剂的制备及其加氢脱硫性能

匡志敏1,龚建议2,杨运泉1,王威燕1,陈来福1,贺 恒1   

  1. (1湘潭大学化工学院,湖南 湘潭411105;2中国石油化工股份有限公司催化剂分公司,北京 100011)

Abstract:

Al-MCM-41 mesoporous molecular sieves were prepared by the azeotropic distillation and ultrasonic dispersive technology using sodium silicate as silica source aluminum sulfate as aluminum source and cetyltrimethyl ammonium bromide as structure-directing agent. By using Al-MCM-41 as supportnickel nitrate and diammonium hydrogen phosphate as raw materialsa series of supported Ni2P catalysts on Al-MCM-41 was prepared via the method of temperature-programmed reduction under ultrasonic oscillation. The catalysts were characterized by FTIRBETXRD and SEM. Hydrodesulfurization of thiophene catalyzed by Ni2P/Al-MCM-41 was carried out in a high pressure autoclave reactor. The experimental results showed that Al-MCM-41 prepared by ultrasonic dispersive technology had a much higher specific surface arealarger pore volume and pore diameter than that prepared by conventional mechanical mixing. The Al-MCM-41 prepared by azeotropic distillation with ultrasonic dispersive technology was also better than that using only ultrasonic dispersive technology. The Ni2P/Al-MCM-41 catalystshydrodesulfurization conversion of thiophene nearly reached 100% at the reaction time 5 hreaction temperature 548 Kand reaction pressure 3.5 MPa.

摘要:

以硅酸钠为硅源、硫酸铝为铝源、十六烷基三甲基溴化铵(CTAB)作模板剂,采用共沸蒸馏与超声波分散技术相结合的方法制备了介孔分子筛Al-MCM-41。以Al-MCM-41为载体、硝酸镍和磷酸氢二氨为原料,采用超声波振荡、程序升温还原法制备了Ni2P/Al-MCM-41催化剂,并对Al-MCM-41Ni2P/Al-MCM-41进行了傅里叶变换红外光谱、比表面积测定、X射线衍射、扫描电镜表征。考察了Ni2P/Al-MCM-41催化剂对噻吩加氢脱硫的催化性能。结果表明:采用超声波制得的Al-MCM-41其比表面积、孔容和孔径明显高于常规搅拌制得的Al-MCM-41,共沸蒸馏制得的Al-MCM-41其比表面积、孔容和孔径高于未共沸蒸馏的Al-MCM-41在反应时间为5 h548 K3.5 MPa条件下,Ni2P/Al-MCM-41催化剂对噻吩加氢脱硫的转化率接近100%

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