Hydroprocessing catalysts and their production
a technology of hydroprocessing catalysts and catalysts, which is applied in the direction of physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, fatty-oils/fats refining, etc., can solve the problems of reducing the density relative to the mixed metal oxide and limiting the relative amount of inorganic constituents present in the phase, so as to reduce the density and limit the relative amount of inorganic constituents
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[0076]In the Examples, X-ray diffraction spectra were collected on a Rigaku Dmax diffractometer with Cu Kα radiation. Thermogravimetry, Dynamic Thermal Analysis, and Mass Spectrometry (TG / DTA / MS) data were collected on a Mettler TGA 851 thermal balance, interfaced with a Balzers Thermostar quadrupole mass spectrometer, which was equipped with a secondary electron multiplier. Weight loss during air oxidation at about 800° C. was monitored both before and after the thermal treatment of the organically treated catalyst precursor to estimate the amount of organic components present in the sample. Also, the sulfided phases can be oxidized to form oxides (a weight loss event), thus allowing estimation of additional weight loss due to retention of the organic component in the sulfide phase.
[0077]For TEM measurements, samples of the sulfided compositions were crushed into pieces (less than about 100 nm thick), dusted onto holey-carbon coated grids, and examined in a bright field imaging mod...
preparation examples
Comparative Example 1: Preparation of NiWO4 and NiMo0.5W0.5O4 (No Organics)
[0079]A metastable hexagonal variant of NiWO4 is formed by a solid-slurry reaction between nickel carbonate and tungstic acid. About 5.93 grams nickel carbonate and about 12.49 grams tungstic acid were added to about 150 mL of water to form a suspension, which was added to a ˜275 mL Weflon™ reaction vessel. The vessel was then heated (in a microwave oven) to about 150° C. for about 6 hours, cooled to about room temperature (about 20-25° C.), and filtered and dried at about 100° C. After drying, the material was heated in a box furnace in air at a ramp rate of about 2° C. / min up to a final temperature of about 300° C. and was held at that temperature for about 4 hours (e.g., to calcine). A portion of this material was labeled as catalyst A. FIG. 1 shows the x-ray diffraction spectrum of this sample, which crystallized in the hexagonal nickel tungstate phase. The Ni1Mo0.5W0.5O4 catalyst, catalyst B, was prepare...
example 8
f Catalysts of Example 1
[0101]The HDN activity of sulfided samples of catalysts 1a, 1a / / N2, 1b, and 1b / / N2, all of which were described in Example 1, were compared against the HDN activity of a sulfided reference sample made from catalyst B. The activities were normalized on a weight basis, relative to the reference, and are shown in Table 5. Because of the relatively low density of these bimetallic oxide-amine hybrid phases, the activities on a relative volume basis were less than that of the reference catalyst.
TABLE 5SampleCompositionRWA1aNiWO4(1,2DACH)2~1.071a / / N2NiWO4(1,2DACH)2 / / N2~1.281bNiWO4(1,2DACH)2 / / citric0.33~0.601b / / N2NiWO4(1,2DACH)2 / / citric0.33 / / N2~1.18
[0102]Table 5 shows that the high temperature inert treatment of the bimetallic oxide-amine precursors, whether citric acid was impregnated or not, improved their activity. The low density, and consequent lower volumetric activity, of these Example 1 precursors tends to make them less preferred than the catalysts of Exampl...
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