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Preparation method of carbon-containing residual oil hydrodemetallization catalyst

A hydrodemetallization and catalyst technology, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of unsatisfactory mechanical strength of catalysts, and prevent The effect of reunion

Active Publication Date: 2016-05-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Preparation method of carbon-containing residual oil hydrodemetallization catalyst
  • Preparation method of carbon-containing residual oil hydrodemetallization catalyst
  • Preparation method of carbon-containing residual oil hydrodemetallization catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Weigh the pore volume as 0.9ml / g and the specific surface area as 220m 2 100 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. Dry the carrier with 150ml containing MoO ...

Embodiment 2

[0037] 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). The temperature of the hydrothermal treatment was 160° C., and the treatment time was 8 hours. Ammonia gas sealing treatment condition is that at first the ammonia gas pressure is 5MPa and seals for 1 hour, then vents part of the ammonia gas, controls the pressure of ammonia gas to be 0.5MPa, and seals for 10 hou...

Embodiment 3

[0039] 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). The temperature of the hydrothermal treatment is 180° C., and the treatment time is 6 hours. The condition of ammonia gas sealing treatment is to feed ammonia gas and nitrogen gas respectively, the partial pressure of ammonia gas in the tube furn...

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Abstract

The invention discloses a preparation method of a carbon-containing residual oil hydrodemetallization catalyst. The preparation method includes the following steps: 1) preparing polyol and / or monosaccharide water solutions in at least two different concentrations, and spray-impregnating an alumina carrier with the water solutions according to the sequence of high concentration to low concentration to form a low-to-high gradient distribution of concentrations of the polyol and / or monosaccharide from exterior to interior of the carrier; 2) performing hydrothermal carbonization treatment to the impregnated alumina carrier in a sealed container and then drying the carrier; 3) impregnating the carrier in the step 2) with an impregnation liquid containing active metal components, placing the impregnated wet material in a pressure-resistant container, and feeding ammonia gas to perform stepwise treatment; and 3) drying the material treated in the step 3) and performing oxygen-free high-temperature treatment to prepare the catalyst. The content of carbon in the catalyst is distributed in a gradient manner, so that active components are easy to sulfurize completely, and the catalyst is significantly improved in demetallization and desulfurization activities.

Description

technical field [0001] The invention belongs to catalyst preparation technology, in particular to a preparation method of a carbon-containing 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...

Claims

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Application Information

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IPC IPC(8): B01J23/883B01J35/10C10G45/08
Inventor 季洪海凌凤香王少军沈智奇杨卫亚王丽华郭长友
Owner CHINA PETROLEUM & CHEM CORP
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