反应 #2195470

ord-ee7ca75d983b482c924ebe2fd1541287

反应方程式

N#N
N2
S.[H][H]
H2S H2
S.[H][H]
H2S H2
c1ccc(C2CCCCC2)cc1
CHB
N#N
N2
c1ccc2c(c1)sc1ccccc12
Dibenzothiophene

反应条件

温度
400°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他inserted into a horizontal quartz tube
  2. 2
    workup.WAITheld there for 2 hours
  3. 3
    温度the catalyst cooled
  4. 4
    其他to 70° C.
  5. 5
    其他At room temperature, the quartz tube was removed
  6. 6
    其他the material transferred into a N2 purged glove box
  7. 7
    workup.ADDITION100 cc of liquid feed, containing 5 wt % dibenzothiophene in decalin
  8. 8
    workup.ADDITIONwas added to the autoclave
  9. 9
    温度the pressure was maintained at 3150 kPa
  10. 10
    温度The temperature was raised to 350° C. at 5-6 deg/min
  11. 11
    workup.WAITwas converted or until 7 hours
  12. 12
    其他A small aliquot of product was removed every 30 minutes
  13. 13
    其他As described in that article, high selectivities to cyclohexylbenzene relative to BP during the desulfurization reaction

实验过程

1.5-2 g of the catalysts of Examples 1-4 were placed in a quartz boat which was in turn inserted into a horizontal quartz tube and placed into a Lindberg furnace. The temperature was raised to 370° C. in about one hour with N2 flowing at 50 cc/m, and the flow continued for 1.5 h at 370° C. No was switched off and 10% H2S/H2 then added to the reactor at 20 cc/m, the temperature increased to 400° C., and held there for 2 hours. The heat was then shut off and the catalyst cooled in flowing H2S/H2 to 70° C., at which point this flow was discontinued and N2 was added. At room temperature, the quartz tube was removed and the material transferred into a N2 purged glove box. Catalysts were evaluated in a 300 cc modified Carberry batch reactor designed for constant hydrogen flow. The catalyst was pilled and sized to 20/40 mesh and one gram was loaded into a stainless steel basket, sandwiched between a layer of mullite beads. 100 cc of liquid feed, containing 5 wt % dibenzothiophene in decalin was added to the autoclave. A hydrogen flow of 100 cc/min was passed through the reactor and the pressure was maintained at 3150 kPa using a back pressure regulator. The temperature was raised to 350° C. at 5-6 deg/min and run until either 50% DBT was converted or until 7 hours was reached. A small aliquot of product was removed every 30 minutes and analyzed by GC. Rate constants for the overall conversion as well as the conversion to the reaction products biphenyl (BP) and cyclohexylbenzene (CHB) were calculated as described by M. Daage and R. R. Chianelli [J. Cat. 149, 414-27 (1994)] and are shown in Table 1. As described in that article, high selectivities to cyclohexylbenzene relative to BP during the desulfurization reaction are a good indication of a catalyst with high hydrodenitrogenation activity, whereas high selectivities of BP relative to CHB indicates a catalyst with high hydrodesulfurization activity.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07513989B1uspto-grants-2009_04