A kind of sulfurized hydrogenation catalyst and its preparation method and application

A hydrogenation catalyst and vulcanization-type technology, applied in physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve problems such as poor controllability, complicated preparation process, and high cost question

Active Publication Date: 2020-05-19
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the defects of low activity, relatively complicated preparation process, poor controllability and high cost of prior art sulfurized hydrogenation catalysts, the present invention provides a new preparation method of sulfurized hydrogenation catalysts and the obtained Sulfurized hydrogenation catalyst and the application of the above-mentioned sulfurized hydrogenation catalyst in hydrodesulfurization and / or hydrodenitrogenation, the method provided by the invention introduces the main agent component and the auxiliary agent component in one step, and the prepared catalyst active group The component is not only highly dispersed, but also fully vulcanized, which finally significantly improves the hydrogenation performance of the catalyst

Method used

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  • A kind of sulfurized hydrogenation catalyst and its preparation method and application
  • A kind of sulfurized hydrogenation catalyst and its preparation method and application
  • A kind of sulfurized hydrogenation catalyst and its preparation method and application

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preparation example Construction

[0025] The present invention provides a kind of preparation method of vulcanization type hydrogenation catalyst, and this method comprises the following steps:

[0026] (1) Mix the dispersant with solution A containing metal salts of Group VIB, metal salts of Group VIII and sulfur source, the solution A is acidic, and the dispersant is a water-soluble organic solvent with a boiling point of 15-90°C , the sulfur source is a sulfur-containing substance that can be hydrolyzed under acidic conditions at 50-100°C;

[0027] (2) contacting the mixture obtained in step (1) with the catalyst carrier at 60-150° C. for 5-30 hours under airtight conditions;

[0028] (3) Calcining the solid material obtained after contacting in step (2) in an inert or reducing atmosphere.

[0029] In the present invention, preferably, the Group VIII metal is cobalt and / or nickel, and the Group VIB metal is molybdenum and / or tungsten.

[0030] In the present invention, preferably, the Group VIB metal salt...

Embodiment 1

[0089] Prepare an aqueous solution containing 0.15mol / L sodium molybdate, 0.06mol / L nickel nitrate, and 0.45mol / L thioacetamide. During stirring, add 2.4mol / L hydrochloric acid 4.0mL dropwise to obtain 40mL solution A. The pH value is 5.0;

[0090] Measure 20mL of absolute ethanol, and add the absolute ethanol dropwise to solution A at a rate of 1mL / min while stirring continuously to form solution B;

[0091] 4.0g of γ-Al with a diameter of 2-5mm 2 o 3 Particles (surface SEM image see figure 1) immersed in 20.0mL of a mixed aqueous solution containing 0.2mol / L cobalt nitrate and 1.0mol / L urea, heat-treated at 80°C for 24 hours, filtered, washed and then dried at 120°C for 4 hours. ℃ calcination for 4 hours to obtain Co-modified alumina support Z-1, the SEM image of Z-1 is as follows figure 2 shown. From figure 2 It can be seen that the surface of the Co-modified alumina support has a large number of network structures, and the network density is listed in Table 2;

[0...

Embodiment 2

[0094] Prepare an aqueous solution containing 0.20 mol / L sodium tungstate, 0.1 mol / L nickel acetate, and 0.60 mol / L thioacetamide. During stirring, add 4.5 mL of 2.4 mol / L hydrochloric acid dropwise to obtain 30 mL of solution A. The pH value is 4.5;

[0095] Measure 30mL of absolute ethanol, and add the absolute ethanol dropwise to solution A at a rate of 1mL / min while stirring continuously to form solution B;

[0096] 4.0g of γ-Al with a diameter of 2-5mm 2 o 3 The particles are immersed in 13.0mL mixed aqueous solution containing 0.1mol / L nickel nitrate and 0.4mol / L urea, heat-treated at 70°C for 18 hours, filtered, washed and then dried at 130°C for 2 hours, in 100mL / min air flow at 550 ℃ roasting for 2 hours to obtain Ni-modified alumina carrier Z-2, the grid density of Z-2 is listed in Table 2;

[0097] Transfer the solution B to the autoclave filled with the alumina carrier Z-2 prepared above, then place the autoclave in a rotary oven (rotating at 80 rpm) and contact...

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Abstract

The invention relates to the field of hydrorefining, and discloses a vulcanization type hydrogenation catalyst, a preparation method and applications thereof. The method comprises: (1) mixing a dispersing agent and a solution A containing a group VIB metal salt, a group VIII metal salt and a sulfur source, wherein the solution A is acidic, the dispersing agent is a water-soluble organic solvent with a boiling point of 15-90 DEG C, and the sulfur source is a sulfur-containing material capable of being hydrolyzed at 50-100 DEG C under an acidic condition; (2) making the mixture obtained in the step (1) contact a catalyst carrier for 5-30 h at a temperature of 60-150 DEG C under a sealed condition; and (3) calcining the solid material obtained in the step (2) in an inert or reducing atmosphere. With the method of the present invention, the main agent component and the auxiliary agent component are introduced in one step, and the active component of the prepared catalyst is highly dispersed and fully vulcanized so as to significantly improve the hydrogenation performance of the catalyst.

Description

technical field [0001] The present invention relates to the field of hydrofining, in particular to a method for preparing a sulfurized hydrogenation catalyst, a sulfurized hydrogenation catalyst prepared by the method and its application in hydrodesulfurization and / or hydrodenitrogenation . Background technique [0002] Hydrogenation technology is the most important means of producing clean oil products, among which efficient hydrogenation catalyst is the core technology of hydrogenation technology. The main active component is VIB group metal W or Mo, the VIII group metal Ni or Co is the auxiliary active component, and γ-A1 2 o 3 or modified γ-A1 2 o 3 The supported catalyst is a hydrogenation catalyst widely used in industry at present. The traditional preparation technology mainly uses impregnation to introduce the oxidized precursor of the active component into the pores of the carrier, and then aging, drying, and roasting to obtain the hydrogenation catalyst. Amon...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C10G45/08
CPCB01J31/0228C10G45/08C10G2300/202
Inventor 韩伟龙湘云李明丰杨清河聂红邵志才
Owner CHINA PETROLEUM & CHEM CORP
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