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Recycling method of inactivated hydrogenation catalyst

A hydrogenation catalyst and catalyst technology, which are applied in the direction of catalyst regeneration/reactivation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as adverse effects, poor economy, and aggregation of active metals, and improve hydrogenation activity. , The effect of improving denitrification performance and dispersion degree

Active Publication Date: 2022-05-03
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of burning charcoal and burning sulfur, not only a large amount of harmful gas is produced, but also high-temperature charcoal burning is likely to cause further accumulation of active metals, reduce the utilization rate of active metals, greatly affect the performance of the regenerated catalyst, and have an adverse effect on the reaction
At present, the relatively small amount of carbon deposits is mainly due to the fact that the aggregation of active metal components (mainly including Group VIII) leads to less research on catalysts with reduced activity. According to the current charcoal regeneration method, it will not only cause waste of vulcanizing agents. , is also unfavorable to the recovery of activity, and the economy is poor

Method used

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  • Recycling method of inactivated hydrogenation catalyst
  • Recycling method of inactivated hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Get deactivated hydrotreating catalyst A, its carbon deposition content is 2.2wt%, active metal component is composed as follows: MoO 3 content of 24.8wt% and NiO content of 4.2wt%, the deactivated catalyst was added to the methyl phosphoric acid ester solution, the weight ratio of methyl phosphoric acid ester to the catalyst was 2:100, the catalyst was put into an atmosphere furnace for heat treatment, and the Under nitrogen, heat up to 400°C, treat at a constant temperature for 2 hours, continue to heat up to 500°C at a heating rate of 15°C / min, treat at a constant temperature for 0.5 hours, cool down to room temperature, and use nickel citrate (citric acid and nickel nitrate according to mole Ratio 1.2:1 configuration) solution impregnation, so that metallic nickel accounts for 3.5% of the weight of the finished catalyst (calculated as nickel oxide). Then put it into an atmosphere furnace for heat treatment, raise the temperature to 200° C. under a nitrogen atmospher...

Embodiment 2

[0031] Take the deactivated hydrotreating catalyst A, add the deactivated catalyst to the dimethyl phosphate solution, the weight ratio of dimethyl phosphate to the catalyst is 3:100, put the catalyst into an atmosphere furnace for heat treatment, and heat up under nitrogen to 400°C, treated at constant temperature for 2 hours, continued to heat up to 530°C at a heating rate of 18°C / min, treated at constant temperature for 0.2 hours, cooled to room temperature, and then immersed in ammonium acetate solution (concentration: 15wt%), the ammonium acetate solution The amount is 10 wt% of the catalyst weight. The catalyst was heat-treated in an air-blast drying oven at 80°C for 3 hours, and the intermediate product was impregnated with a solution of nickel citrate (citric acid and nickel nitrate were configured at a molar ratio of 1:1), so that the metal nickel accounted for 2.0% of the weight of the finished catalyst (according to Nickel oxide calculation). Then put it into an at...

Embodiment 3

[0033] Get the deactivated hydrogenation treatment catalyst A, add the glycerin solution of dioctyl phosphate to the deactivated catalyst, the weight ratio of dioctyl phosphate and the catalyst is 3:100, the catalyst is put into the atmosphere furnace and carry out heat treatment, under nitrogen The temperature was raised to 380°C at low temperature, treated at constant temperature for 3 hours, continued to heat up to 550°C at a heating rate of 15°C / min, treated at constant temperature for 0.3 hours, cooled to room temperature, and the intermediate product was impregnated with EDTA nickel solution (EDTA and nickel nitrate according to the molar ratio 1.2:1 configuration) solution impregnation, so that metallic nickel accounts for 4.0% of the weight of the finished catalyst (calculated as nickel oxide). Then put it into a vacuum oven for heat treatment with a vacuum degree of -0.08MPa, raise the temperature to 150°C, and treat at a constant temperature for 3 hours to obtain cata...

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Abstract

The invention discloses a regeneration and utilization method of an inactivated hydrogenation catalyst, which comprises the following steps: (1) uniformly mixing the inactivated hydrogenation catalyst with a phosphorus-containing compound solution, and then carrying out first heat treatment; and (2) uniformly mixing the sample obtained in the step (1) with a solution containing VIII group metal components, and carrying out second heat treatment to obtain the catalyst. The catalyst obtained by the method disclosed by the invention is in a sulfurized state and can be directly used, so that the step of sulfurization treatment before use can be omitted, and the activity of the catalyst is relatively high.

Description

technical field [0001] The invention relates to a method for preparing a catalytic material, in particular to a method for preparing a catalyst by using an inactivated catalyst as a raw material. Background technique [0002] Hydrogenation catalysts are key to the production of clean fuel oils and other chemical feedstocks from crude oil. During the hydrogenation process, the catalyst will be deactivated due to various reasons, mainly including: the active metal on the catalyst changes due to long-term operation, the pore structure of the catalyst changes due to the carbon deposit on the catalyst, impurities in the raw oil (such as Catalyst irreversible deactivation caused by metal nickel, vanadium) deposition, etc. Among these phenomena, the influence of carbon deposition is the most obvious. Deactivated hydrotreating catalysts typically contain 3-15% by weight of carbon deposits which result in a reduction in catalyst surface area and pore volume. At present, catalysts ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J38/48B01J38/52B01J38/02B01J27/30C10G45/08C10G47/04
CPCB01J38/485B01J38/52B01J38/02B01J27/30C10G45/08C10G47/04C10G2300/202C10G2300/701C10G2300/703Y02P20/584
Inventor 杨涛徐黎明高玉兰佟佳杨占林
Owner CHINA PETROLEUM & CHEM CORP