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Nano hierarchical pore SiO2@Cu/Ni core-shell material as well as preparation method and application thereof

A multi-level porous, nano-level technology, applied in catalyst activation/preparation, nanotechnology, nanotechnology, etc., can solve the problems of high preparation cost and poor stability of precious metal active centers

Active Publication Date: 2020-11-27
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a nano-scale porous SiO 2 in view of the technical problems of poor stability of noble metal active centers and high preparation costs in existing fuel oil desulfurization catalysts. 2 @Cu / Ni core-shell materials and their preparation methods and applications, specifically to provide a hierarchical porous SiO with cheap transition metals as reactive centers 2 @Cu / Ni core-shell material and its preparation method, as well as the application of the core-shell material in the study of the catalytic cleavage of sulfide C-S bonds in fuel oil, experiments show that the core-shell material exhibits higher selectivity and better desulfurization It has the characteristics of simple production process, low equipment requirements, cheap and easy-to-obtain raw materials, etc.

Method used

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  • Nano hierarchical pore SiO2@Cu/Ni core-shell material as well as preparation method and application thereof
  • Nano hierarchical pore SiO2@Cu/Ni core-shell material as well as preparation method and application thereof

Examples

Experimental program
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preparation example Construction

[0033] A Nanoscale Hierarchical Porous SiO 2 The preparation method of @Cu / Ni core-shell material, comprises the following steps:

[0034] 1) Mix ethyl orthosilicate and ethanol at a volume ratio of 1:(30-40) and prepare a tetraethyl orthosilicate solution, mix ammonia water and water at a volume ratio of 1:(6-6.5) and prepare to obtain ammonia aqueous solution;

[0035] 2) Mix ethyl orthosilicate solution with ammonia solution and stir at 20-30°C for 20-28h, then centrifuge, and wash the solid product obtained by centrifugation until neutral, then dry at 100-120°C for 10 -12h, and then calcined at 545-555°C for 4-7h to obtain nano-scale spherical SiO 2 ; Wherein, the volume ratio between the ethyl orthosilicate in the ethyl orthosilicate solution and the ammonia in the ammonia solution is 1:(0.5-1.5);

[0036] 3) Nanoscale spherical SiO 2 Mix with water at a mass volume ratio of 0.18-0.23g / 65mL to prepare a dispersion, and then mix the dispersion with (0.048-0.052)mol·L ...

Embodiment 1

[0042] A Nanoscale Hierarchical Porous SiO 2 The preparation method of @Cu / Ni core-shell material, comprises the following steps:

[0043] 1) Mix 4mL tetraethyl orthosilicate with 140mL ethanol to obtain tetraethyl orthosilicate solution; mix 4mL ammonia water with 25mL water to obtain ammonia solution;

[0044] 2) Mix ethyl tetrasilicate solution with ammonia solution and stir at 25°C for 24h, then centrifuge, and wash the solid product obtained by centrifugation to neutrality, then dry at 110°C for 12h, and then place in a tube furnace Medium to 2°C·min -1 The heating rate was heated to 550 ° C, and the constant temperature was calcined for 5 hours to obtain nano-scale spherical SiO 2 ;

[0045] 3) 0.2g nanoscale spherical SiO 2 Add to 65mL water and ultrasonically disperse evenly to get SiO 2 Dispersions;

[0046] 4) to SiO 2 Add 7.2mL 0.05mol L to the dispersion -1 CuSO 4 ·5H 2 O solution, after stirring at 30°C for 1 hour, add 0.12g reducing agent iron powder, a...

Embodiment 2

[0051] In this embodiment, SiO prepared in Example 1 2 @Cu / Ni core-shell material is used as a desulfurization catalyst to catalyze the C-S bond breaking reaction of 4,6-dimethyldibenzothiophene. The specific experimental process is as follows:

[0052] The reaction activity test of the catalyst was carried out in a fixed-bed reactor, and the dosage of the catalyst was 20 mg. Before the desulfurization reaction, the catalyst was heated in 800 °C H 2 Reduction in the atmosphere for 3h, so that the Cu center in the catalyst is replaced by Cu 2 Exist in the form of O, then cool to room temperature, will contain 1% methanol, 1% H 2 o 2 , 5% 4,6-DMDBT benzene solution mixture is introduced into the preheater, then flows into the reactor containing the catalyst, and stays at a specific reaction temperature for 65min. The experimental results are as follows figure 2 shown. From figure 2 It can be seen that even under mild conditions, the desulfurization rate and selectivity o...

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Abstract

The invention relates to a nano hierarchical pore SiO2@Cu / Ni core-shell material as well as a preparation method and application thereof. The preparation method comprises the following steps of: firstly, preparing a nano spherical SiO2 dispersion liquid, and sequentially mixing the nano spherical SiO2 dispersion liquid with a copper source solution and a reducing agent to obtain brick red precipitate; calcining the brick red precipitate to obtain a core-shell material SiO2@Cu; and finally, preparing a dispersion liquid containing SiO2@Cu and polyvinyl alcohol, mixing the dispersion liquid witha nickel source, and sequentially carrying out heating stirring, oven drying and high-temperature calcination to obtain the nano hierarchical pore SiO2@Cu / Ni core-shell material. Compared with the prior art, the preparation method disclosed by the invention has the advantages of simple process, low cost, good stability, easiness in popularization and the like, and the prepared core-shell materialcan be used as an efficient breaking catalyst for C-S bonds in 4, 6-DMDBT and shows excellent desulfurization performance.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and relates to a nano-scale porous SiO 2 @Cu / Ni core-shell materials and their preparation methods and applications. Background technique [0002] Hierarchical porous materials have the characteristics of rich pore structure, high specific surface area and large pore capacity, and have broad application prospects in various fields such as optics, magnetism, electricity, adsorption, separation, catalysis, energy storage, and biotechnology. On the one hand, because of the multi-level porous core-shell material, it has obvious advantages. The shell layer has a stabilizing effect on the core: after covering the outer surface of nanoparticles such as metals or oxides with a stable shell layer to form a core-shell structure, it will make The stability of the core nanoparticles is greatly improved, and they can adapt to many reactions under high temperature conditions, which significantly improves th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J35/10B01J37/16B01J37/18B01J37/03B01J37/08B82Y30/00B82Y40/00C10G11/02C10G11/04
CPCB01J23/755B01J37/16B01J37/18B01J37/031B01J37/088C10G11/02C10G11/04C10G2300/202B01J35/397B01J35/695
Inventor 王磊孙梦刘倩袁国良李书珍马莹莹
Owner SHANGHAI INST OF TECH
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