Ex-situ pre-vulcanization method for deep vulcanization of hydrogenation catalyst
A technology of hydrogenation catalyst and external presulfurization, which is applied in the fields of chemical instruments and methods, catalyst activation/preparation, catalyst protection, etc., can solve the problems such as the mismatch of start-up and operation of hydrogenation reactors, and achieve reduced start-up time and good activity , the effect of improving safety
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Embodiment 1
[0031] The FHUDS-5 catalysts for diesel hydrogenation in Table 1 were presulfided outside the reactor.
[0032] (1) The vulcanizing agent (elemental sulfur, the dosage is 90% of the theoretical sulfur requirement of the diesel hydrogenation catalyst), the vulcanization aid (a mixture of industrial soybean oil and kerosene in a weight ratio of 1:1, the dosage is the diesel hydrogenation catalyst FHUDS- 5% by weight) and mix uniformly to obtain presulfurized raw materials; presulfurized raw materials and diesel hydrogenation catalysts are uniformly mixed;
[0033] (2) Heat the mixed material in step (1) at 140°C for 1 hour.
[0034] (3) The intermediate material in step (2) is treated with the low fraction gas of the hydrogenation unit (the volume content of hydrogen sulfide is 12%), the amount of hydrogen sulfide quoted is 15% of the theoretical sulfur demand of the diesel hydrogenation catalyst, and the processing pressure 3.0MPa, treated at 320°C for 1 hour.
[0035] (4) Th...
Embodiment 2
[0039] FHFHUDS-5 in Table 1 was precured ex-situ.
[0040] (1) The vulcanizing agent (elemental sulfur, the dosage is 115% of the theoretical sulfur requirement of the diesel hydrogenation catalyst), the vulcanization aid (a mixture of industrial soybean oil and gasoline at a weight ratio of 2:1, the dosage is the diesel hydrogenation catalyst FHFHUDS- 9% of 5 weight) mixed uniformly to obtain the presulfurized raw material; the presulfurized raw material and the diesel hydrogenation catalyst were uniformly mixed;
[0041] (2) Heat-treat the mixed material in step (1) at 150°C for 0.5 hours.
[0042] (3) The material obtained in step (2) is treated with hydrogenation unit circulating hydrogen exhaust gas (hydrogen sulfide volume content is 6%), and the hydrogen sulfide quoted amount is 5% of the theoretical sulfur requirement of the diesel hydrogenation catalyst, Pressure 0.6MPa, heat treatment at 180°C for 1 hour.
[0043] (4) Load citric acid and lubricating oil into the m...
Embodiment 3
[0047] Evaluation tests were performed on the deeply sulfided external presulfided catalysts obtained in Examples 1-2 and the catalysts obtained in Comparative Examples 1-2. Mainly compare the initial activation temperature of different external presulfided catalysts (the initial activation temperature is based on the obvious release of water in the presence of hydrogen, corresponding to the lowest boosting temperature of the hydrogenation reactor), and the relative activity after activation.
[0048] The test method for the initial activation temperature is: after drying with nitrogen at 90°C for 5 hours, in the presence of 0.2MPa (gauge pressure) and hydrogen, gradually increase the temperature. The temperature at which water is obviously collected from the material at the outlet of the device is the initial activation temperature.
[0049] The activation process conditions are: at 320°C, in the presence of 6MPa (gauge pressure) and hydrogen, activate for 15 hours.
[0050] ...
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