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Slurry bed residual oil hydrogenation catalyst and preparation method thereof

A technology of hydrogenation catalyst and bed residue, which is applied in the direction of refining to remove heteroatoms, etc. It can solve the problems of low dispersion of active metals and the limitation of catalyst activity improvement, and achieve high catalytic hydrodesulfurization activity, long service life, good dispersion effect

Inactive Publication Date: 2016-10-05
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the specific surface area of ​​activated carbon-supported residual oil hydrogenation catalysts prepared by conventional methods is mostly less than 500m 2 / g, the activity of the catalyst is limited, such as the Chinese patent CN99113278.5
The slurry bed residual oil hydrogenation catalyst prepared by conventional methods has high specific surface area and active metal content, but the active metal dispersion is not high, and the activity of the catalyst is also limited, such as Chinese patent CN97121844.7

Method used

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  • Slurry bed residual oil hydrogenation catalyst and preparation method thereof

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preparation example Construction

[0026] In order to make the specific surface area of ​​the catalyst larger, the dispersity of the supported metal higher, the catalytic hydrodesulfurization activity higher, and it is suitable for processing inferior residue oil with (Ni+V) metal content greater than 150 μg / g, the present invention provides a slurry. A method for preparing a catalyst for hydrogenation of residual oil in a state bed, comprising the following steps:

[0027] 1) After the activated carbon is washed with hydrochloric acid, the activated carbon is oxidized at 400-600°C;

[0028] 2) prepare a dipping solution, the molar ratio of terephthalic acid, nickel nitrate, urea and ammonium nitrate in the dipping solution is 2:1:2.5-5:1-5;

[0029] 3) The impregnation solution obtained in step 2) is impregnated on the surface of the activated carbon treated in step 1) by the equal volume impregnation method, and then transferred to the pressure solution bomb for crystallization for 24-32 hours after the cryst...

Embodiment a

[0041] The present embodiment provides a method for preparing a slurry bed residual oil hydrogenation catalyst, comprising the following steps:

[0042] 1) Wash the activated carbon (wood activated carbon and coconut shell activated carbon) with hydrochloric acid (use hydrochloric acid with a concentration of 20%, wash the activated carbon in a boiling state for 5 hours, and then rinse with deionized water, the mass ratio of hydrochloric acid and activated carbon is 5:1 ), and then under the condition of 400 ° C, the activated carbon was treated with a nitrogen-oxygen mixed gas with an oxygen content of 1% for 1 hour to make it undergo an oxidation reaction;

[0043] 2) prepare a dipping solution, the molar ratio of terephthalic acid, nickel nitrate, urea and ammonium nitrate in the dipping solution is 2:1:2.5:1;

[0044] 3) The impregnation solution obtained in step 2) was impregnated on the surface of the activated carbon treated in step 1) by the equal volume impregnation m...

Embodiment b

[0048] The present embodiment provides a method for preparing a slurry bed residual oil hydrogenation catalyst, comprising the following steps:

[0049] 1) Activated carbon (apricot shell activated carbon and coal-based activated carbon) is washed with hydrochloric acid (using hydrochloric acid with a concentration of 35%, the activated carbon is washed in a boiling state for 24h, and then rinsed with deionized water, and the mass ratio of hydrochloric acid and activated carbon is 20: 1), and then under the condition of 600 ° C, the activated carbon is treated with a nitrogen-oxygen mixed gas with an oxygen content of 5% for 3 hours to carry out an oxidation reaction;

[0050] 2) prepare a dipping solution, the molar ratio of terephthalic acid, nickel nitrate, urea and ammonium nitrate in the dipping solution is 2:1:5:5;

[0051] 3) The impregnation solution obtained in step 2) was impregnated on the surface of the activated carbon treated in step 1) by the equal volume impreg...

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Abstract

The invention discloses a slurry bed residual oil hydrogenation catalyst and a preparation method thereof. The preparation method comprises the following steps: performing hydrochloric acid washing on active carbon, performing high-temperature partial oxidation; preparing an impregnation solution; employing an equivalent-volume impregnation method for impregnating the active carbon, performing steps of standing, crystallization, washing and drying to obtain nickel salt hydrotalcite microcrystalline; putting the nickel salt hydrotalcite microcrystalline in a Mo salt solution for being stirred, filtering and washing the material to obtain the green solid particles, and drying and roasting the green solid particles to obtain the slurry bed residual oil hydrogenation catalyst. According to the invention, the specific surface of the catalyst is larger, dispersity of the loaded metal is higher, and the catalytic hydrogenation desulfurization activity is higher.

Description

technical field [0001] The invention relates to a catalyst used in a residual oil hydrodesulfurization process, in particular to a slurry bed residual oil hydrodesulfurization catalyst. Background technique [0002] The residual oil hydrogenation technology can further process and utilize the residual oil remaining in the atmospheric and vacuum units of the refinery, and the economic effect is obvious. The slurry bed residue hydrogenation technology is favored by scholars at home and abroad because it can process the inferior residue with (Ni+V) metal content greater than 150μg / g. The core of this technology is to develop a highly active slurry-bed residue hydrogenation catalyst, which has become a research hotspot at home and abroad. [0003] The activity of the slurry bed residue hydrogenation catalyst mainly depends on the specific surface area and the dispersity of active metals. It is found that the activity of the catalyst can be effectively improved only by increasin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/883C10G45/08
Inventor 张春光赵愉生谭青峰程涛于双林赵元生周志远张志国范建光崔瑞利刘佳澎由慧玲王燕周漪
Owner PETROCHINA CO LTD