Preparation method of high-activity inferior diesel oil hydrorefining catalyst

A technology for hydrorefining and inferior diesel oil, applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc. Reduced agglomeration ability, high reactivity and strong penetration ability, weakening the effect of interaction

Active Publication Date: 2012-04-25
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this series of catalysts has good hydrofining performance, it requires high metal content, which increases the cost of the catalyst, and compared with the comparison catalyst, the desulfurization activity has a small increase
[0006] Compared with the traditional hydrogenation catalysts with bimetallic components, the existing hydrogenation catalysts containing trimetallic components have improved activity, but the degree of improvement is limited, and their activity is still low

Method used

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  • Preparation method of high-activity inferior diesel oil hydrorefining catalyst
  • Preparation method of high-activity inferior diesel oil hydrorefining catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 10g of shaped γ-Al 2 o 3 Put the carrier into a 100mL autoclave, add 7.2mL and 3.2mL of sodium tungstate solution and sodium molybdate solution with a concentration of 1.5mol / L respectively, then add 13mL of hydrochloric acid with a concentration of 2.4mol / L, and stir evenly , add 10mL ethanol (volume ratio of ethanol to water in the final autoclave is 1:5), 7.5mL concentration is 2.0mol / L ammonium fluoride and 12.5mL BS-12 (molar ratio WMo:BS-12=1: 0.5), finally add 6.6mL of water to make the total solvent in the autoclave 60mL, heat up to 150°C, rotate and stir for 24h, cool to room temperature, filter the suspension, wash with water, and dry the obtained solid product at 110°C for 2h , 550 ℃ roasting 4h, get MoW / Al 2 o 3 ;

[0032] MoW / Al 2 o 3 Put it into the autoclave again, add 50 mL of nickel nitrate solution with a concentration of 0.1 mol / L, stir evenly, add 10 mL of ethanol (the volume ratio of ethanol to water in the final autoclave is 1:5) and 1....

Embodiment 2

[0034] Weigh 10g of molded γ-Al 2 o 3 Put the carrier into a 100mL autoclave, add 7.2mL and 3.2mL of sodium tungstate solution and sodium molybdate solution with a concentration of 1.5mol / L respectively, then add 13mL of hydrochloric acid with a concentration of 2.4mol / L, and stir evenly , add 12mL of ethanol (the volume ratio of ethanol to water in the final autoclave is 1:4), 7.5mL of ammonium fluoride with a concentration of 2.0mol / L and 12.5mL of zwitterionic surfactant BS-12 (the molar ratio is WMo: BS-12=1:0.5), finally add 4.6mL of water to make the total amount of solvent 60mL, heat up to 150°C, rotate and stir for 24 hours, cool to room temperature, filter the suspension, wash with water, and obtain a solid product at 110°C Drying for 2h, calcination at 550°C for 4h to obtain MoW / Al 2 o 3 ;

[0035] MoW / Al 2 o 3 Put it into the autoclave again, add 50 mL of nickel nitrate solution with a concentration of 0.1 mol / L, stir evenly, add 10 mL of ethanol (the volume r...

Embodiment 3

[0037] Weigh 10g of molded γ-Al 2 o 3 Put the carrier into a 100mL autoclave, add 7.2mL and 3.2mL of sodium tungstate solution and sodium molybdate solution with a concentration of 1.5mol / L, respectively, and then add 13.0mL of hydrochloric acid with a concentration of 2.4mol / L. Stirring, add 10mL ethanol (volume ratio of ethanol to water in the final autoclave is 1:5), 7.5mL concentration is 2.0mol / L ammonium fluoride and 12.5mL zwitterionic surfactant BS-12 (molar ratio is WMo : BS-12=1: 0.5), finally add 6.6mL of water to make the total amount of solvent 60mL, heat up to 150°C, rotate and stir for 24h, cool to room temperature, filter the suspension, wash with water, and the solid product obtained at 110 ℃ drying for 2h, 550℃ calcination for 4h to get MoW / Al 2 o 3 ;

[0038] MoW / Al 2 o 3 Put it into the autoclave again, add 50 mL of nickel nitrate solution with a concentration of 0.1 mol / L, stir evenly, add 10 mL of ethanol (the volume ratio of ethanol to water in the...

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Abstract

The invention relates to a preparation method of a high-activity inferior diesel oil hydrorefining catalyst. The method comprises steps that: a molding carrier and a salt solution of VIB metals are added into an autoclave; an inorganic acid is adopted as a precipitating agent; a zwitterionic surfactant and a fluorine-containing compound are adopted as a composite dispersant; an alcohol solvent and water are added into the autoclave, and a solvent thermal reaction is carried out for 12-36h under a temperature of 100-200 DEG C; a suspension obtained through the reaction is filtered; a filter cake is washed, dried, and baked, such that a fluorine-containing bimetallic catalyst is obtained; the bimetallic catalyst and a salt solution containing VIII metals are placed in the autoclave; an anionic surfactant is adopted as a dispersant, a certain amount of an alcohol solvent and water are added into the autoclave, and the mixture is subject to solvent thermal reaction for 12-36h under a temperature of 100-200 DEG C; the reaction product is filtered, washed, dried, and baked, such that the inferior diesel oil hydrorefining catalyst is obtained. With the method provided by the invention, the obtained catalyst has relatively high hydrodesulfurization activity and hydrodenitrogenation activity.

Description

technical field [0001] The invention relates to a preparation method of a hydrogenation catalyst capable of achieving higher desulfurization and denitrogenation activities, in particular to a preparation method of a high-activity inferior diesel hydrofinishing catalyst, which belongs to the technical field of hydrofinishing catalyst preparation. Background technique [0002] With the increasingly stringent requirements of environmental protection regulations in the world, the demand for low-sulfur and low-nitrogen clean diesel oil is increasing day by day. Hydrogenation technology has become the most effective means for large-scale production of clean diesel oil. key in . The supported catalyst with Group VIB metal W or Mo as the main agent, Group VIII metal Ni or Co as the auxiliary agent, and alumina as the carrier is currently the most widely used hydrofining catalyst. Generally speaking, for the desulfurization reaction-based reaction process, the hydrogenation active c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/132B01J37/08C10G45/08
Inventor 范煜祝伟孙国方鲍晓军石冈
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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