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Method for preparing high-activity residual oil hydrodemetalation catalyst

A technology of hydrodemetallization and residual oil hydrogenation, which is applied in metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., and can solve problems such as unsatisfactory mechanical strength of catalysts , to achieve the effect of promoting the reaction

Active Publication Date: 2016-04-27
SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because the shaped support has not been roasted, the mechanical strength of the catalyst is not ideal

Method used

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  • Method for preparing high-activity residual oil hydrodemetalation catalyst
  • Method for preparing high-activity residual oil hydrodemetalation catalyst
  • Method for preparing high-activity residual oil hydrodemetalation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh the pore volume as 0.9ml / g and the specific surface area as 220m2 100 grams of gamma-phase cylindrical strip-shaped alumina carrier / g is put into the spray rolling pot, and in the rotating state, spray and impregnate 25 ml of xylitol aqueous solution with a mass concentration of 40% to the carrier in the rolling pot in the form of atomization ; Then continue to spray and impregnate the alumina carrier with 40ml of xylitol aqueous solution with a mass concentration of 20%; finally continue to spray and impregnate the alumina carrier with 40ml of xylitol aqueous solution with a mass concentration of 10%. After impregnation, the alumina carrier was transferred into an autoclave, and the autoclave was placed in an oven at 180° C. for 9 hours under autogenous pressure for carbonization treatment, and then cooled naturally to room temperature. The alumina carrier after hydrothermal treatment was dried at 120° C. for 3 hours. The dried carrier was filled with 150ml conta...

Embodiment 2

[0032] Same as Example 1, except that the alumina carrier is a clover strip, 30ml of sorbitol aqueous solution with a mass concentration of 30% is used for the first spray and impregnation, and 50ml of sorbitol with a mass concentration of 10% is used for the second spray and impregnation. For the aqueous alcohol solution, use 20ml of sorbitol aqueous solution with a mass concentration of 5% for the third spraying and dipping. The temperature during carbonization treatment is 200°C, and the carbonization time is 8 hours. MoO in impregnating solution 3 8g / 100ml (molybdenum source comes from ammonium molybdate), NiO1.2g / 100ml (nickel source comes from nickel chloride), urea 20g / 100ml. The temperature of the hydrothermal treatment was 160° C., and the treatment time was 8 hours. The hydrodemetallization catalyst C2 of the present invention was prepared, and the properties of the catalyst are shown in Table 1.

Embodiment 3

[0034] With embodiment 1, just adopt four times of spray impregnation, use 20ml mass concentration to be the aqueous solution of mannitol of 50% during the first spray impregnation, use 40ml mass concentration to be 30% sorbitol during the second spray impregnation 20ml of sorbitol aqueous solution with a mass concentration of 20% was used for the third spray and dipping, and 20ml of a sorbitol aqueous solution with a mass concentration of 10% was used for the fourth spray and dip. During the carbonization treatment, the temperature was 240° C., and the carbonization time was 12 hours. MoO in impregnating solution 3 12g / 100ml (molybdenum source comes from ammonium molybdate), NiO1.8g / 100ml (nickel source comes from nickel chloride), urea 30g / 100ml. The temperature of the hydrothermal treatment is 180° C., and the treatment time is 6 hours. The hydrodemetallization catalyst C3 of the present invention was prepared, and the properties of the catalyst are shown in Table 1.

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Abstract

The invention discloses a method for preparing a high-activity residual oil hydrodemetalation catalyst. The method comprises the following steps: 1) at least two polyol and / or monosaccharide aqueous solutions with different concentration are prepared, according to a decreasing concentration sequence, spray leaching is carried out on an alumina carrier, increasing gradient distribution of the polyol and / or monosaccharide concentration on the carrier from outer to inner; 2) hydro-thermal charing processing is carried out on the dipped alumina carrier in a sealed container, and then is dried; and 3) an active ingredient and urea-containing aqueous solution is used for dipping the alumina carrier in the step 2), the dipped material is converted to the sealed container for hydro-thermal processing, then is dried, and is performed with anoxic high temperature processing to obtain the hydrodemetalation catalyst. The carbon content in the prepared catalyst presents gradient distribution, the active ingredient is easily and completely sulfurated, distribution of the active metal ingredient on a surface is uniform, and the demetallization activity of the catalyst is obviously increased.

Description

technical field [0001] The invention relates to a preparation method of a highly active residual oil hydrogenation demetallization catalyst. Background technique [0002] At present, the most common hydrogenation catalysts are generally supported catalysts with alumina, silica, etc. as the carrier, and Co, Ni, Mo, W and other metals as active components. The active components are loaded on the carrier by impregnation or kneading, and then dried and calcined to obtain the catalyst. When the impregnated wet agent dries, the active components in the impregnating liquid will easily form larger active species particles in the pores of the carrier as the solvent gradually evaporates, causing some pores in the carrier to be blocked, while the solvent evaporates during the evaporation process. The migration of active components will also make the distribution of active components uneven, which will eventually affect the activity of the catalyst. In addition, during the calcination...

Claims

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Application Information

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IPC IPC(8): B01J23/883C10G45/08
Inventor 王少军季洪海凌凤香沈智奇杨卫亚王丽华郭长友
Owner SINOPEC DALIAN RES INST OF PETROLEUM & PETROCHEM
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