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N-rGO loaded copper-nickel bimetallic monatomic catalyst as well as preparation and application thereof

A catalyst and bimetallic technology, which is applied in the field of copper-nickel bimetallic single-atom catalysts, can solve problems such as few researches, and achieve the effects of safe and easy-to-obtain raw materials, simple preparation process, and simple preparation process

Active Publication Date: 2019-11-22
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, few studies have been conducted on the selective in situ hydrogenation coupled catalytic oxidation of Cu / Ni bimetallic single-atom supports on N-rGO for C-S bond selectivity via isolated single-atom catalytic cracking of C-S bonds of sulfides in fuels. The technique of fracture has not been reported so far

Method used

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  • N-rGO loaded copper-nickel bimetallic monatomic catalyst as well as preparation and application thereof
  • N-rGO loaded copper-nickel bimetallic monatomic catalyst as well as preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] A copper-nickel bimetallic single-atom catalyst supported by N-rGO is prepared by the following method:

[0056] Weigh 0.3g of graphene and mix it with 70mL (0.5mol / L) hydrochloric acid, sonicate in an ice bath for 1.5 hours, drop 300 μL of aniline into the suspension and stir for 0.3 hours to obtain the first suspension;

[0057] Slowly add 2.0mL (1.5mol / L) of (NH 4 ) 2 S 2 o 8 And stirred in ice bath for 8 hours, filtered and washed 3 times, and dried under vacuum at 363K for 4 hours. The obtained composite was heated to 973K in an Ar atmosphere at a heating rate of 3.2K / min in a tube furnace and calcined at a constant temperature for 1 hour to obtain N-rGO;

[0058] Disperse 100 mg of N-rGO in 50 mL of water and sonicate for 1 h to obtain a homogeneous suspension. Then, by dropwise adding Na 2 CO 3 (0.5mol / L) solution adjusts solution pH to 9.5, is recorded as the second suspension;

[0059] Polyvinyl alcohol was dissolved in 200mL water to obtain an aqueous ...

Embodiment 2

[0064] Weigh 0.3g of graphene and mix it with 70mL (0.5mol / L) hydrochloric acid, sonicate in an ice bath for 1.5 hours, drop 300 μL of aniline into the suspension and stir for 0.3 hours to obtain the first suspension;

[0065] Slowly add 2.2mL (1.5mol / L) of (NH 4 ) 2 S 2 o 8 And stirred in ice bath for 10 hours, filtered and washed 3 times, and dried under vacuum at 363K for 5 hours. The obtained composite was heated to 973K at a heating rate of 3.2K / min in an Ar atmosphere in a tube furnace and calcined at a constant temperature for 2 hours to obtain N-rGO;

[0066] Disperse 102 mg of N-rGO in 50 mL of water and sonicate for 1 h to obtain a homogeneous suspension. Then, by dropwise adding Na 2 CO 3 (0.5mol / L) solution adjusts solution pH to 10.0, is recorded as the second suspension;

[0067] Polyvinyl alcohol was dissolved in 200mL water to obtain an aqueous solution of polyvinyl alcohol containing 0.3vol% polyvinyl alcohol;

[0068] Dissolve copper nitrate and nicke...

Embodiment 3

[0071] The activity experiment of the catalyst was carried out in the reactor, with 20mg of the catalyst obtained in Example 1——Cu / Ni-N-rGO with a Cu / Ni loading of 0.8wt% (wherein 0.4wt% Cu, 0.4wt% Ni) catalyzed Cleaves the C-S bond in 4,6-DMDBT. Before the desulfurization reaction, the prepared samples were heated at 523K in H 2 (18mol%H in the mixed gas 2 , flow rate: 26mL / min) for 1 hour reduction. After cooling to room temperature, add 1% methanol, 1% O 2 , a gas mixture of 5% 4,6-DMDBT and the balance He (flow rate 40mL / min), then heated to 393K, and stabilized at the reaction temperature for 45 minutes.

[0072] Experiments have found that when the reaction temperature is 393K, the desulfurization rate of 4,6-DMDBT and the selectivity to sulfone respectively reach 100%, which proves that the catalytic system is an ideal deep desulfurization catalytic system.

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Abstract

The invention relates to an N-rGO loaded copper-nickel bimetallic monatomic catalyst as well as a preparation and application thereof. The catalyst comprises a carrier N-rGO and copper and nickel which are loaded on the carrier and have the radius smaller than that of the carrier, and the preparation method comprises the following steps of 1) mixing graphene and hydrochloric acid, and then addinganiline; 2) adding a (NH4) 2S2O8 solution, mixing, filtering, drying and roasting to obtain the N-rGO; 3) adding the N-rGO into water, and adding a Na2CO3 solution to obtain a second turbid liquid; 4)mixing the mixed aqueous solution of copper nitrate and nickel nitrate with the polyvinyl alcohol aqueous solution to obtain a mixed solution; and 5) adding the mixed solution into the second turbidliquid, and sequentially mixing, filtering, drying and roasting to obtain the catalyst. The catalyst is used for the selective C-S bond cleavage reaction of 4, 6-DMDBT in the catalytic cracking fuel.Compared with the prior art, the catalyst disclosed by the invention is high in reaction activity, simple in preparation process and outstanding in desulfurization effect on the compounds, such as 4,6-DMDBT, etc., in the fuel oil.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to an N-rGO-supported copper-nickel bimetallic single-atom catalyst and its preparation and application. Background technique [0002] With the improvement of environmental quality requirements, the intensification of smog weather and the deterioration of crude oil, fuel oil is facing challenges in terms of environmental protection and production technology, and the key scientific problem of super-clean hydrogenation of fuel oil is how to solve the process of hydrodesulfurization (HDS) For the steric hindrance of 4,6-dimethyldibenzothiophene (4,6-DMDBT), non-hydrodesulfurization must focus on highly selective oxidative cleavage of carbon-sulfur bonds. For typical sulfur compounds in fuel oil, such as benzothiophenes (BTs) and dibenzothiophenes (DBTs), relative hydrogenation reaction rate: BT>DBT>>4,6-DMDBT, relative oxidation reaction rate: 4 ,6-DMDBT>DBT>>BT, whe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C10G47/12
CPCB01J27/24C10G47/12C10G2300/202B01J35/393B01J35/23
Inventor 王磊刘倩孟凡帅谢大祥左宁
Owner SHANGHAI INST OF TECH
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