Hydrodenitrification catalyst as well as preparation method and application thereof
A hydrodenitrogenation and catalyst technology, which is applied in catalyst activation/preparation, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc. The effect of processability, improved state of existence, good desulfurization and carbon residue removal
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Embodiment 1
[0037] Weigh 2000.0g of alumina dry rubber powder, add 40.0g of citric acid and 50.0g of scallop powder, mix well, add 1800.0g of aqueous solution containing 4.0% acetic acid mass fraction, roll for 15.0min, and use clover with a diameter of 2.0mm Orifice extruded strips. After drying at 130°C for 6.0h, it was calcined at 650°C for 3.0h. The calcined carrier is designated as S-0.
[0038] Weigh 68.0g of ammonium heptamolybdate and 30.0g of 25wt% ammonia water to prepare a 180mL aqueous solution, and the solution is designated as MQ-1. 200g S-0 was impregnated with 180mL of MQ-1, dried at 140°C for 4.0h, and then calcined at 450°C for 2.0h to obtain 3 The catalyst intermediate is denoted as MA-1.
[0039] Weigh 50 g of MA-1, 200 g of carbon tetrachloride, and 2.0 g of nickel tetracarbonyl into an autoclave with a volume of 500 mL, feed ether gas, maintain a pressure of 4.0 MPa, and a temperature of 200 ° C for 5 h. Afterwards, the temperature was lowered to 90°C, carbon mon...
Embodiment 2
[0043] The preparation process of the carrier S-0 and the MA-1 of the molybdenum-containing catalyst intermediate is the same as in Example 1.
[0044] Weigh 50.0 g of MA-1, 150 g of carbon tetrachloride, and 2.0 g of dicobalt octacarbonyl into an autoclave with a volume of 500 mL, feed ether gas, maintain a pressure of 4.0 MPa, and a temperature of 200°C for 5 hours of reaction. Afterwards, the temperature was lowered to 90° C., carbon monoxide was introduced, the pressure was raised to 12.0 MPa, and the reaction was carried out for 5 hours. The catalyst was taken out and dried at 120° C. for 2 hours. The obtained material was designated as MT-2.
[0045] Weigh 8.2 g of cobalt nitrate hexahydrate, 10.0 g of EDTA, and dissolve them in 50.0 mL of aqueous solution. The obtained solution is denoted as BQ-2. Impregnate MT-2 with BQ-2 and dry at 120° C. for 4.0 h. The obtained catalyst is denoted as BQ-2. for TC-2.
[0046] Take 10.0 g TC-2 and put it into a tubular reactor for pr...
Embodiment 3
[0048] The preparation process of the carrier S-0 and the MA-1 of the molybdenum-containing catalyst intermediate is the same as in Example 1.
[0049] Weigh 50.0 g of MA-1, 150 g of carbon tetrachloride, and 2.0 g of nickel tetracarbonyl, and add them into an autoclave with a volume of 500 mL, feed in methyl ether gas, maintain a pressure of 4.0 MPa, and a temperature of 200 ° C for 5 h. Afterwards, the temperature was lowered to 90° C., carbon monoxide was introduced, the pressure was raised to 12.0 MPa, and the reaction was carried out for 5 hours. The catalyst was taken out and dried at 120° C. for 2 hours. The obtained material was designated as MT-3.
[0050] Weigh 8.2 g of nickel nitrate hexahydrate, 2.0 g of ethylenediamine, dissolve in 50.0 mL of water, and record the obtained solution as BQ-3, impregnate MT-3 with BQ-3, and dry at 120 ° C for 4.0 h to obtain the catalyst Recorded as TC-3.
[0051] Take 10.0g TC-3, put it into a tubular reactor, and carry out the pre...
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