Method for preparing supported oil product hydrodesulphurization catalyst with solvothermal method at normal pressure

A solvothermal and hydrodesulfurization technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. Agglomeration and other problems, to achieve the effect of high catalytic hydrodesulfurization performance, cheap raw materials, high activity and stability

Inactive Publication Date: 2014-12-17
NORTHEAST GASOLINEEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ni2P catalyst is usually synthesized by temperature programmed reduction (Ni(NO3)2 6H2 O) and diammonium hydrogen phosphate ((NH4)2HPO4) as the precursor, the process is simple but requires a high The reduction temperature (generally 600-750 ℃), not only wastes a lot of energy in the synthesis process, but also high temperature will cause the agglomeration of the active phase state, and put forward higher requirements for the choice of carrier (such as anatase TiO2 carrier cannot withstand such a high temperature)
The synthesis of Ni2P catalyst by pyrolysis of hypophosphite is usually made of nickel chloride (NiCl2·6H2O) and sodium hypophosphite ( The mixed salt of NaH2PO2 · H2O) is the precursor, which can be generated under nitrogen atmosphere without high temperature treatment Ni2P, but the synthesized catalyst contains a large amount of phosphate impurities, so the hydrodesulfurization activity of the catalyst prepared by this method is not high
The traditional solvothermal method is to synthesize under high pressure under the alkaline condition of ammonia water, or use expensive trioctylphosphine as the phosphorus source, and synthesize under normal pressure under the liquid phase environment of oleylamine. Due to the limitation of cost and reaction conditions, it is difficult to Realize the requirements of large-scale industrial production

Method used

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  • Method for preparing supported oil product hydrodesulphurization catalyst with solvothermal method at normal pressure
  • Method for preparing supported oil product hydrodesulphurization catalyst with solvothermal method at normal pressure
  • Method for preparing supported oil product hydrodesulphurization catalyst with solvothermal method at normal pressure

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Experimental program
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Effect test

Embodiment 1

[0022] Add nickel acetylacetonate, triphenylphosphine and MCM-41 mesoporous sieve into tri-n-octylamine according to a certain metering ratio, and stir at room temperature until fully mixed. Among them, the mass ratio of nickel acetylacetonate, triphenylphosphine, MCM-41 mesoporous sieve and tri-n-octylamine is 1:2:0.67:32.

[0023] The second step, reaction preparation catalyst:

[0024] Add the slurry obtained in the first step into a stirred reactor at normal pressure, heat it to 330 °C at a rate of 2 °C per minute in a nitrogen flow of 100 mL / min under stirring conditions, and keep the temperature at this temperature for 3 hours. Cool down to room temperature, and finally with 10% (V / V) O 2 / N 2 Mixed gas passivation for 1 hour.

[0025] The third step, filtering, washing and drying:

[0026] The passivated slurry was filtered under reduced pressure with a sand core funnel, and the filter cake after washing was washed at 50°C with a mixed solution of ethanol and carbon...

Embodiment 2

[0032] Add nickel acetylacetonate, triphenylphosphine and MCM-41 mesoporous sieve into tri-n-octylamine according to a certain metering ratio, and stir at room temperature until fully mixed. Among them, the mass ratio of nickel acetylacetonate, triphenylphosphine, MCM-41 mesoporous sieve and tri-n-octylamine is 1:6:0.67:32.

[0033] The second step, reaction preparation catalyst:

[0034]Add the slurry obtained in the first step into a stirred reactor at normal pressure, heat it to 330 °C at a rate of 2 °C per minute in a nitrogen flow of 100 mL / min under stirring conditions, and keep the temperature at this temperature for 3 hours. Cool down to room temperature, and finally with 10% (V / V) O 2 / N 2 Mixed gas passivation for 1 hour.

[0035] The third step, filtering, washing and drying:

[0036] The passivated slurry was filtered under reduced pressure with a sand core funnel, and the filter cake after washing was washed at 50°C with a mixed solution of ethanol and carbon ...

Embodiment 3

[0042] Add nickel acetylacetonate, triphenylphosphine and MCM-41 mesoporous sieve into tri-n-octylamine according to a certain metering ratio, and stir at room temperature until fully mixed. Among them, the mass ratio of nickel acetylacetonate, triphenylphosphine, MCM-41 mesoporous sieve and tri-n-octylamine is 1:10:0.67:32.

[0043] The second step, reaction preparation catalyst:

[0044] Add the slurry obtained in the first step into a stirred reactor at normal pressure, heat it to 330 °C at a rate of 2 °C per minute in a nitrogen flow of 100 mL / min under stirring conditions, and keep the temperature at this temperature for 3 hours. Cool down to room temperature, and finally passivate with O2 / N2 gas mixture containing 10% oxygen (V / V) for 1 hour.

[0045] The third step, filtering, washing and drying:

[0046] The passivated slurry was filtered under reduced pressure with a sand core funnel, and the filter cake after washing was washed at 50°C with a mixed solution of etha...

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Abstract

The invention discloses a method for preparing supported oil product hydrodesulphurization catalyst with solvothermal method at normal pressure. The method comprises the following steps: adding acetylacetone nickel, triphenyl phosphine and MCM-41 interface confucius screen to tri-n-octylamine, and evenly stirring a mixture at room temperature; adding slurry obtained in the first step to a normal-pressure stirring reactor, heating the slurry to 330 DEG C with an increment of 2 DEG C per minute in nitrogen flow of 100mL / min; keeping the temperature constantly for 3 hours, and reducing the temperature to the room temperature, finally, passivating the slurry for 1 hour by O2 / N2 mixing gas containing 10% of oxygen; filtering the passivated slurry under reduced pressure by a sand-core hopper; washing an obtained filter cake with mixed solution of ethanol and carbon tetrachloride based on volume ratio of 1: 1 at 50 DEG C; and drying the filter cake at 100 DEG C and tabletting the filter cake so as to obtain a catalyst finished product. According to the invention, the prepared supported oil product hydrodesulphurization catalyst disclosed by the invention has the advantages of soft condition, little dependence on equipment, little impurity and high desulphurization rate.

Description

technical field [0001] The invention belongs to the technical field of oil hydrodesulfurization catalysts, and in particular relates to a method for preparing a load-type oil hydrodesulfurization catalyst by solvothermal method under normal pressure. Background technique [0002] As people continue to pay attention to environmental issues, environmental protection regulations have become more and more strict on the sulfur content in fuel oil. Fuel oil desulfurization technology has gradually shifted to the field of deep and ultra-deep desulfurization, but the current commercial transition metal sulfide hydrodesulfurization (HDS) catalysts have been difficult to meet this requirement. Therefore, improving the original sulfide catalysts and finding new high-efficiency substitutes have become the focus of recent research by researchers. Ni 2 P is a material with high hydrodesulfurization activity discovered in recent years. Under the same test conditions, Ni 2 P / SiO 2 Cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/76C10G45/12
Inventor 宋华李锋代敏柳艳修张娇静赵丽
Owner NORTHEAST GASOLINEEUM UNIV
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