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Double-metal-sulfide catalyst with high hydrodeoxygenation activity and preparation method thereof

A hydrodeoxygenation and catalyst technology, which is applied in the direction of physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problem that the bimetallic synergy cannot get the maximum effect, and achieve excellent catalytic activity. High hydrodeoxygenation activity and effect of increasing specific surface area

Inactive Publication Date: 2014-07-16
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the synergistic catalytic model of bimetallic sulfide catalysts, it is inferred that most of the Ni- or Co-sulfides in the catalyst prepared by the one-step hydrothermal method will be wrapped in the catalyst, and the synergistic effect of bimetallic cannot get the maximum effect. to play

Method used

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  • Double-metal-sulfide catalyst with high hydrodeoxygenation activity and preparation method thereof
  • Double-metal-sulfide catalyst with high hydrodeoxygenation activity and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Dissolve 1.39g of ammonium molybdate in 150ml of deionized water, add 1.81g of thiourea and stir to dissolve, then pour it into a 300ml reaction kettle, close the lid of the kettle, stir and mix, react at 200°C for 12 hours, cool down to 40°C, and open the reaction cauldron lid. Dissolve 0.17g of nickel nitrate in 30ml of deionized water, add 0.08g of thiourea to dissolve, then add this solution into the previously opened reaction kettle, close the lid of the kettle, stir and mix at 300r / min, and react at 200°C for 12 hours. After the reaction, a black precipitate was obtained, which was washed with water and alcohol, and dried in a vacuum oven at 40° C. for 5 hours.

[0031] Add 86.5 g of n-dodecane, 13.5 g of p-cresol and 0.60 g of the catalyst prepared above in the autoclave. Raise to 300°C, adjust the rotation speed to 900r / min, hydrogen pressure to 4.0MPa, and continue the reaction for 6 hours. The product was analyzed by Agilent 6890 / 5973N GC-MS, and the conversi...

Embodiment 2

[0033] Dissolve 1.39g of ammonium molybdate in 150ml of deionized water, add 1.81g of thiourea and stir to dissolve, then pour it into a 300ml reaction kettle, close the lid of the kettle, stir and mix, react at 200°C for 12 hours, cool down to 50°C, and open the reaction cauldron lid. Dissolve 0.50g of nickel nitrate in 30ml of deionized water, add 0.23g of thiourea to dissolve, then add this solution into the previously opened reaction kettle, close the lid of the kettle, stir and mix at 300r / min, and react at 200°C for 12 hours. After the reaction, a black precipitate was obtained, which was washed with water and alcohol, and dried in a vacuum oven at 40° C. for 5 hours.

[0034] Add 86.5 g of n-dodecane, 13.5 g of p-cresol and 0.60 g of the catalyst prepared above in the autoclave. Raise to 300°C, adjust the rotation speed to 900r / min, hydrogen pressure to 3.0MPa, and continue the reaction for 6 hours. The product was analyzed by Agilent 6890 / 5973N GC / MS, and the conversi...

Embodiment 3

[0036] Dissolve 1.39g of ammonium molybdate in 150ml of deionized water, add 1.81g of thiourea and stir to dissolve, then pour it into a 300ml reaction kettle, close the lid of the kettle, stir and mix, react at 200°C for 12 hours, cool down to 50°C, and open the reaction The cauldron should. Dissolve 0.50g of cobalt nitrate in 30ml of deionized water, add 0.23g of thiourea to dissolve, then add this solution into the previously opened reaction kettle, close the lid of the kettle, stir and mix at 300r / min, and react at 200°C for 12 hours. After the reaction, a black precipitate was obtained, which was washed with water and alcohol, and dried in a vacuum oven at 40° C. for 5 hours.

[0037] Add 86.5 g of n-dodecane, 13.5 g of p-cresol and 0.10 g of the catalyst prepared above in the autoclave, install the high-pressure reaction device, remove the air in the autoclave, and then rise from room temperature at a rate of 10 °C / min. To 250°C, adjust the rotation speed to 900r / min, h...

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Abstract

The invention relates to a preparation method for a double-metal-sulfide catalyst. Soluble molybdate and nickel salt or cobalt salt serves as a raw material, thiourea or thioacetamide serves as a sulfur source, and a Ni(Co)-S / MoS2 catalyst is prepared through a two-step hydrothermal method. The method particularly comprises the following steps: MoS2 is prepared in a high pressure reactor through the hydrothermal method first, then the nickel salt or cobalt salt and the sulfur source are added into the reactor of the obtained MoS2 to be evenly mixed, the reactor is sealed and heated, a reaction is conducted for a certain period of time, and Ni-S or Co-S is deposited on the MoS2, so that the Ni(Co)-S / MoS2 catalyst is prepared. The preparation method is characterized in that the specific area of the Ni(Co)-S / MoS2 catalyst prepared through the two-step hydrothermal method is large, high temperature vulcanization is not required in the preparation process, the preparation condition is mild, the catalyst is used for hydrodeoxygenation, a target product has high yield and good repeatability, and hydrodeoxygenation activity of the catalyst is high.

Description

technical field [0001] The invention relates to a bimetallic sulfide catalyst with high hydrodeoxygenation activity and a preparation method thereof, which can be used in the catalytic hydrodeoxygenation reaction of oxygen-containing compounds in bio-oil and real bio-oil, and belongs to the technical field of catalytic refining of biomass energy. Background technique [0002] With the continuous depletion of non-renewable fossil energy such as coal, oil and natural gas and the severe environmental problems caused by their utilization, the development and preparation of renewable clean petroleum alternative energy has attracted widespread attention from all over the world. Bio-oil, a liquid fuel obtained by high-temperature pyrolysis of biomass, has a net increase of carbon dioxide and harmful gases (SO x , NO x ) and heavy metal content are almost zero, so it is recognized as the most potential and ideal renewable new oil alternative energy in the world. Its development and...

Claims

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Application Information

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IPC IPC(8): B01J27/051C10G45/04
Inventor 王威燕杨运泉李路张锟仵奎
Owner XIANGTAN UNIV
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