Sulfurized hydrogenation catalyst and its preparation method and application
A hydrogenation catalyst and sulfide-type technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of low activity of sulfide-type hydrogenation catalysts, complicated preparation process, poor controllability, etc. , to achieve the effect of high utilization rate of active metal, low preparation cost and excellent degree of sulfidation
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[0023] The invention provides a kind of preparation method of vulcanization type hydrogenation catalyst, this method comprises the following steps:
[0024] (1) Prepare solution A containing VIB group metal salt, sulfur source and optionally a water-soluble organic dispersant, the sulfur source is a sulfur-containing substance that can be hydrolyzed at 50-100° C. under acidic conditions, and the solution A The pH value is 1-8;
[0025] (2) aging the solution A described in step (1) at 20-120° C. for 0.5-48 hours to obtain an aging product;
[0026] (3) using the aging product to impregnate the catalyst carrier;
[0027] (4) Roasting the impregnated solid material in step (3) in an inert or reducing atmosphere;
[0028] The method also includes the step of introducing Group VIII metal elements in step (1) and / or step (3).
[0029]In the present invention, solution A is adjusted to an appropriate pH value in step (1), and then aging treatment is carried out under the conditio...
Embodiment 1
[0061] (1) Prepare 40mL of a solution containing 2.4mol / L sodium molybdate and 8.0mol / L thioacetamide, add dropwise (speed is 1mL / min) 4.5mL absolute ethanol in the process of constant stirring, and then During the stirring process, 2.4mol / L hydrochloric acid was added dropwise to adjust the pH value to 6 to obtain solution A;
[0062] (2) aging the solution A obtained in step (1) at 60° C. for 24 hours to obtain an aging product;
[0063] (3) Add 9.0 g of nickel acetate to the aging product described in step (2), add water to constant volume or heat and concentrate to 48 mL, impregnate 60.0 g of γ-Al with a diameter of 1-5 mm in this solution 2 o 3 Granules (liquid absorption rate 0.8mL / g), immersion time is 1 hour;
[0064] (4) The solid product impregnated in step (3) was dried at 50° C. for 3 hours in a nitrogen atmosphere, and then 2 In the atmosphere, the temperature was raised to 300°C at a rate of 5°C / min and kept for 1h, and then the temperature was raised to 360°C...
Embodiment 2
[0073] (1) Prepare 40 mL of a solution containing 2.4 mol / L of sodium molybdate, 0.9 mol / L of nickel acetate, and 9.0 mol / L of thioacetamide, and add it dropwise during constant stirring (at a speed of 1 mL / min) 3mL of acetone, and then during stirring, dropwise add 2.4mol / L hydrochloric acid to adjust the pH value to 6 to obtain solution A;
[0074] (2) aging the solution A obtained in step (1) at 60° C. for 24 hours, adding water to constant volume or heating and concentrating to 48 mL to obtain an aging product;
[0075] (3) impregnate 60.0g of gamma-Al with a diameter of 1-5mm with the aging product described in step (2) 2 o 3 Granules (liquid absorption rate 0.8mL / g), immersion time is 2 hours;
[0076] (4) The solid product impregnated in step (3) was dried at 50° C. for 3 hours in a nitrogen atmosphere, and then 2 In the atmosphere, the temperature was raised to 300°C at a rate of 5°C / min and kept for 1h, and then the temperature was raised to 360°C at a rate of 20°C...
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