A kind of preparation method of bulk phase hydrogenation treatment catalyst

A hydrogenation treatment and catalyst technology, applied in the direction of physical/chemical process catalysts, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of affecting the distribution of hydrogenation active metals and increasing the pores of catalysts Solve problems such as capacity and active metal aggregation, and achieve the effect of improving ultra-deep hydrodesulfurization performance, reasonable catalyst pore structure, and improving interaction

Active Publication Date: 2019-02-22
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The bulk phase hydrogenation catalyst disclosed by CN102049265A adds ammonium bicarbonate during the coprecipitation process, and the bulk phase hydrogenation catalyst disclosed by CN102451703A adds carbon dioxide during the coprecipitation process to generate carbonate or bicarbonate. It releases a certain amount of gas during the roasting process. Under the impact of the gas, the pore volume and specific surface area of ​​the catalyst are increased, so that more metal active sites are exposed on the surface of the catalyst, but this method will cause some pores to collapse. , the pore distribution is dispersed, the mechanical strength is reduced, and the active metal is locally aggregated, and the exposed metal active sites are limited
The co-precipitation method adopted above will make the distribution of different hydrogenation active metals difficult to control, thereby affecting the distribution of different hydrogenation active metals and reducing the interaction between active metals. At the same time, the content of surface active metals in the catalyst is relatively low. Small and low active center density, which ultimately affects the ultra-deep hydrodesulfurization performance of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Dissolve nickel chloride and aluminum chloride solutions in purified water respectively to prepare mixed solution A. The weight concentration of NiO in mixed solution A is 19g / L, Al 2 O 3 The weight concentration of 13g / L. Dissolve ammonium metatungstate and aluminum chloride solutions in purified water respectively to prepare mixed solution B. WO in mixed solution B 3 The weight concentration is 39g / L, Al 2 O 3 The weight concentration of 13g / L. Ammonia water with a concentration of 10wt% was added to solution A under stirring, the gel forming temperature was maintained at 60°C, the pH value was controlled at 7.8 at the end, and the gel forming time was controlled at 60 minutes to generate a slurry I containing nickel and aluminum precipitates. Add 500mL of purified water into the reaction tank, add 10wt% ammonia water and solution B into the reaction tank in parallel flow, keep the gel forming temperature at 60℃, and control the pH value at 7.8 during the gel forming re...

Embodiment 2

[0047] According to the method of Example 1, add the nickel nitrate, aluminum nitrate, and zirconium oxychloride solution to the dissolution tank 1 according to the component content ratio of the catalyst B in Table 1, to prepare the working solution A, and add it to the dissolution tank 2. Prepare working solution B with aluminum nitrate and ammonium metatungstate. Ammonia water with a concentration of 12wt% was added to Solution A under stirring, the gel forming temperature was maintained at 45°C, the pH value was controlled at 8.0 at the end, and the gel forming time was controlled at 50 minutes to generate a slurry I containing nickel and aluminum precipitates. Add 600mL of purified water into the reaction tank, add 12wt% ammonia water and solution B into the reaction tank in parallel, keep the gel forming temperature at 50℃, and control the pH value at 7.6 during the process of the gel forming reaction, and the gel time control In 60 minutes, a slurry II containing tungste...

Embodiment 3

[0049] According to the method of Example 1, add nickel chloride, aluminum chloride, and phosphoric acid solution to the dissolution tank 1 according to the component content ratio of the catalyst C in Table 1 to prepare working solution A, and add chlorine to the dissolution tank 2. Prepare working solution B with aluminum and ammonium metatungstate. Ammonia water with a concentration of 8wt% was added to solution A under stirring, the gel forming temperature was maintained at 50°C, the pH value was controlled at 7.6 at the end, and the gel forming time was controlled at 60 minutes to generate a slurry containing nickel and aluminum precipitates. Add 1000mL purified water into the reaction tank, add 8wt% ammonia water and solution B into the reaction tank in parallel flow, keep the gelation temperature at 55℃, and control the pH value at 8.0 during the gelation reaction and control the gelation time In 60 minutes, a slurry II containing tungsten and aluminum precipitates was f...

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Abstract

The present invention discloses a bulk phase hydrotreating catalyst preparation method, wherein the catalyst comprises hydrogenation activity components such as W, Ni and Mo, and alumina. The preparation method comprises: preparing a nickel-aluminum precipitate slurry I by using an acid type precipitation method; preparing a tungsten-aluminum precipitate slurry II by using a parallel flow precipitation method; mixing the two slurries; aging; carrying out a hydrothermal treatment with water vapor, and adding urea; beating with MoO3, uniformly mixing, and soaking in a solution containing an organic compound; and molding and carrying out other steps to prepare the hydrotreating catalyst. The bulk phase hydrotreating catalyst of the present invention is especially suitable for the super-deep hydrodesulfurization and denitrification reaction of the diesel oil distillate.

Description

Technical field [0001] The invention relates to a preparation method of a hydroprocessing catalyst, in particular to a preparation method of a high-activity bulk hydroprocessing catalyst. Background technique [0002] At present, crude oil is becoming increasingly heavier and degraded worldwide, coupled with the continuous development of the world economy and increasingly stringent environmental regulations, it is necessary to produce a large amount of light and clean fuels. The development and use of ultra-low sulfur or even sulfur-free gasoline and diesel is the trend of clean fuel development worldwide. The use of traditional hydrodesulfurization catalysts can also achieve deep desulfurization or even ultra-deep desulfurization of diesel by increasing the severity of the reaction, such as increasing the reaction temperature, hydrogen partial pressure, or reducing the reaction space velocity, but the increase in reaction temperature will cause the product color Deterioration a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/888B01J35/10C10G45/08
Inventor 王海涛徐学军刘东香冯小萍
Owner CHINA PETROLEUM & CHEM CORP
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