Hydrogenation catalyst precuring method

A hydrogenation catalyst and pre-sulfiding technology, which is applied in catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of complex preparation, high cost, and solvent flammability hazards, and achieve simple preparation. , low price, full and effective effect of vulcanization process

Inactive Publication Date: 2007-07-11
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It involves the complexity of preparation, the flammability of solvents, the harm to human body and the high cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Commercial cobalt molybdenum catalyst, MoO 3 is 15%, CoO is 3.2%, and the carrier is γ-Al 2 o 3 , diameter 1.6mm, water absorption 0.5mL / g catalyst. The catalyst was broken into 20-40 mesh for later use, weighed 5.00g of the catalyst, added 4mL of 50wt% ammonium thiosulfate solution, stirred evenly, soaked at room temperature for 4 hours, put it in an oven and dried at 90°C for 2 hours to obtain a presulfurized catalyst 7.50g,

[0022] Pack 1.50 g of the obtained presulfided catalyst into a tubular reactor. Under 1 MPa hydrogen, the hydrogen flow rate is 2 L / h, from room temperature to 300 ° C in 140 minutes, and the temperature is kept at 300 ° C for 60 minutes. The activated catalyst is fed with 1.5% The model feedstock oil of thiophene dissolved in n-nonane, the temperature, hydrogen pressure and flow rate remain unchanged, and the mass space velocity is 7.2h -1 . The obtained conversion rate of thiophene hydrodesulfurization was 99.3%.

Embodiment 2

[0024] Weigh 5.00g of commercial cobalt-molybdenum catalyst, add 4mL of 50wt% ammonium thiosulfate solution, stir evenly, soak at room temperature for 5 minutes, put it in an oven at 90°C and dry for 2 hours to obtain 7.50g of presulfided catalyst.

[0025] Pack 1.50 g of the obtained presulfided catalyst into a tubular reactor. Under 1 MPa hydrogen, the hydrogen flow rate is 2 L / h, from room temperature to 300 ° C in 140 minutes, and the temperature is kept at 300 ° C for 60 minutes. The activated catalyst is fed with 1.5% The model feed oil of thiophene dissolved in n-nonane, the temperature, hydrogen pressure and flow rate remain unchanged, and the mass space velocity is 7.2h -1 . The obtained conversion rate of thiophene hydrodesulfurization was 98.6%.

[0026] Table 1

[0027] Example 1

[0028] The impregnation needs to ensure a certain period of time, so that the vulcanizing agent can penetrate deep into the pores of the catalyst, so that the active compon...

Embodiment 3

[0030] Weigh 5.00g of commercial cobalt-molybdenum catalyst, add 3mL of 1.5 times (by volume) diluted 50WT% ammonium thiosulfate solution, stir evenly, soak at room temperature for 4 hours, dry in vacuum at room temperature, and the drying time is 10 hours to obtain presulfurized The catalyst 6.65g.

[0031] 1.33 g of the obtained presulfided catalyst was loaded into a tubular reactor, under 1 MPa of hydrogen, from room temperature to 300 °C in 140 minutes, kept at 300 °C for 40 minutes, and decreased to 260 °C in 20 minutes, with a hydrogen flow rate of 2 L / h. The activated catalyst was fed with 1.5% thiophene dissolved in n-nonane model raw material oil, the reaction pressure was 1MPa, the reaction temperature was 260°C, the hydrogen flow rate was 2L / h, and the hydrogen-to-oil ratio was 200. The conversion rate of hydrodesulfurization of thiophene was 77.4%.

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Abstract

The invention relates to a method for pre-vulcanizing hydrogen catalyst, wherein it comprises that: immerging the hydrogen catalyst at oxidation state with oxidation state water solution, while the density of solution is 5wt%-55wt%, immerges for 5min-4h at room temperature, and while the density of solution is 55wt%-70wt%, immerges for 5min-4h at 40-90Deg. C; drying the immerged catalyst at room temperature-90Deg. C at vacuum or normal pressure, for 1-10h. The invention has simple process, while the catalyst activity is higher than the catalyst vulcanized by hydrogen sulfide.

Description

technical field [0001] The invention relates to a presulfurization method of a hydrogenation catalyst. Background technique [0002] Catalysts used for hydrorefining or hydrodesulfurization usually need to convert oxidized metals into highly active and stable metal sulfides before use. This process is called catalyst presulfidation. [0003] At present, the vast majority of pre-sulfurization methods adopt in-vehicle pre-sulfurization methods, including wet and dry methods. Among them, wet pre-sulfurization (liquid phase pre-sulfurization) is after the catalyst is filled, hydrogen (or hydrogen nitrogen) is introduced and the temperature is programmed. , at a certain temperature, the vulcanizing agent (such as CS) is carried by light oil, etc. 2 、CH 3 -S-CH 3 or CH 3 -S-S-CH 3 etc.) to inject sulfurized oil into the reaction system for vulcanization. Dry presulfurization (gas phase presulfurization) is to inject H in the presence of circulating hydrogen (or hydrogen nitr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/20C10G45/08
Inventor 李学宽葛军吕占军王建国
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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