Hydroprocessing catalysts and their production
A technology of hydroprocessing and catalyst, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, catalyst protection, etc.
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Embodiment 1
[0048] Ni was prepared according to the procedure described in U.S. Patent Application Publication No. 2007 / 0090023 1 Mo 0.5 W 0.5 o 4 combination. The Ni 1 Mo 0.5 W 0.5 o 4 Pellet vulcanization. The furnace is used to contain approximately 10 vol% H 2 Flow of S (~200cm 3 / min) hydrogen purge for about 15 minutes. Place these pellets in the same flow (~200cm 3 / min)~10vol%H 2 S (the margin is H 2 ) from ambient temperature (about 20-25°C) to about 400°C in about 45 minutes and held at about 400°C for about 2 hours. These pellets are then cooled and flowed (~200cm 3 / min)~10vol%H 2 S (the margin is H 2 ) at ambient temperature for approximately 30 minutes. Use the furnace with flow (~300cm 3 / min) nitrogen purge for about 30 minutes. Finally, these pellets are placed in a flow (~50cm 3 / min)~1vol%O 2 (the balance being He) overnight and then removed from the furnace.
[0049] 4 to 5 passivated sulfide Ni using an agate mortar and pestle 1 Mo 0.5 W 0.5 T...
Embodiment 2
[0051] performed involving fresh Ni 1 Mo 0.5 W 0.5 o 4 Serial Time-Temperature-Transition Study of Vulcanization of Compositions. Pellets of fresh oxide were prepared again according to US Patent Application Publication No. 2007 / 0090023. In all cases oxide pellets were prepared and subjected to TEM examination as described above. Image a randomly selected area in an oxide sample and use a Gatan CCD TM Camera and Gatan's Digital Micrograph TM v.2.5 software plots their position on the TEM grid. through the flowing (~20cm 3 / min)~10vol%H 2 S (the margin is H 2 ) at approximately 2 °C / min to heat all TEM grids to vulcanize them. Vulcanization time and temperature were varied in each case to better evaluate Ni x S and MoS 2 / WS 2 Particles formed. Details of each vulcanization study are described below.
[0052] In the first study, TEM grids of fresh oxides were sealed in a reactor at ambient temperature with a flowing (~50 cm 3 / min) nitrogen purge for about 30 m...
Embodiment 3
[0056] Re-preparation of Ni using the aforementioned procedure 1 Mo 0.5 W 0.5 o 4 and in a flowing (~20cm 3 / min)~10vol%H 2 S (the margin is H 2 ) to about 400°C for about 2 hours. The vulcanized material was prepared and examined in TEM as described above. Conventional TEM observations consistently reveal that with Ni x S particle-adjacent curved MoS 2 / WS 2 Particles and Ni-depleted in the catalyst x Relatively straight (non-curved) MoS in the S region 2 / WS 2 particles (see Figure 6 ). Ni was confirmed by TEM tilt experiments x S particles and MoS 2 / WS 2 Relationship between particle curvatures. Figure 7 Poor Ni x Typical straight MoS formed in the S region 2 / WS 2 particle form. These two interpenetrating MoS 2 / WS 2 The structure further confirms that these particles are in Ni-poor catalysts x The tendency of the S region to grow in a relatively straight (non-curved) structure (see Figure 7 ). Figure 8 Show next to Ni x Curved MoS formed by...
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