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Yolk-shell bifunctional catalyst, preparation method thereof and application thereof in preparation of ethylene glycol through glucose hydrogenolysis

A dual-functional catalyst and tungsten oxide technology, which is applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve problems affecting catalyst stability, easy agglomeration, and easy loss of metal particles

Inactive Publication Date: 2021-07-09
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the supported catalysts used above have a significant disadvantage: the metal active centers are directly exposed on the surface of the carrier, resulting in the easy loss of metal particles during the reaction process and easy agglomeration at high temperatures, which affects the stability of the catalyst.

Method used

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  • Yolk-shell bifunctional catalyst, preparation method thereof and application thereof in preparation of ethylene glycol through glucose hydrogenolysis
  • Yolk-shell bifunctional catalyst, preparation method thereof and application thereof in preparation of ethylene glycol through glucose hydrogenolysis
  • Yolk-shell bifunctional catalyst, preparation method thereof and application thereof in preparation of ethylene glycol through glucose hydrogenolysis

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preparation example Construction

[0038] The present invention provides the preparation method of the Yolk-shell structure bifunctional catalyst described in above-mentioned technical scheme, comprises the following steps:

[0039] 1) mixing an aqueous template solution with a noble metal salt solution and an aqueous ascorbic acid solution to obtain a noble metal colloid solution, the template being CTAB;

[0040] 2) adjusting the noble metal colloidal solution to alkaline to obtain an alkaline noble metal colloidal solution;

[0041] 3) Mix the alkaline noble metal colloid solution with orthosilicate to carry out silica gel polymerization reaction, mix the obtained reaction solution with the organosilane precursor solution, and separate the solid and liquid to obtain noble metal @SiO 2 YSNSs;

[0042] 4) Roasting the noble metal @ silicon dioxide YSNSs;

[0043] 5) Ultrasonic dispersion of the calcined product and tungsten source aqueous solution to obtain noble metal @W-SiO 2 YSNSs;

[0044] 6) The nob...

Embodiment 1

[0066] 1) Add 0.12g CTAB into a three-necked flask containing 45mL deionized water, heat it from room temperature to 95°C under stirring and keep it for 30min, then add 5mL of K with a molar concentration of 0.02mol / L 2 PdCl 4 Solution, continue to stir until the solution turns into a uniform orange-yellow color, add dropwise 1.7mL of ascorbic acid aqueous solution with a molar concentration of 0.1mol / L, and continue stirring for 30min after the addition to obtain a metal Pd colloidal solution;

[0067] 2) Add 2 mL of NaOH solution with a molar concentration of 0.5 mol / L to the metal Pd colloid solution obtained in step 1), adjust the pH value of the solution to 10-11, then add 0.4 mL of TEOS to it, react for 3 hours and then add 0.3 mL BTME, centrifuged and dried the solid product at 60 °C overnight to obtain Pd@SiO 2 YSNSs;

[0068] 3) The Pd@SiO obtained in step 2) 2 YSNSs were placed in a muffle furnace, heated to 500°C at a rate of 5°C / min and roasted for 3 hours to ...

Embodiment 2～3

[0073] The bifunctional catalyst with yolk-shell structure was prepared according to the scheme of Example 1, except that the amount of ammonium tungstate aqueous solution used in Examples 2-4 was 1 mL and 5 mL respectively.

[0074] figure 1 (b), (c), and (d) are Pd@WO loaded with tungsten content of 0.5wt% (Example 2), 1.5wt% (Example 1) and 2.5wt% (Example 3) x -MSiO 2 TEM images of YSNSs, as can be seen from (b), (c) and (d), the Pd@WO prepared by the present invention x -MSiO 2 YSNSs have a complete yolk-shell structure, the particle size of the nanoparticles is about 80nm, the thickness of the cavity and shell is about 50nm and 15nm, and the Pd particles in the cavity are about 13nm. with unloaded tungsten oxide figure 1 (a) By comparison, it can be found that the nanoparticles loaded with tungsten oxide still maintain the yolk-shell structure, indicating that the loaded tungsten oxide will not destroy the support structure.

[0075] Table 1 Pd@WOx-MSiO with diffe...

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Abstract

The invention provides a Yolk-shell structure bifunctional catalyst which comprises a shell and a movable inner core wrapped in a cavity formed by the shell, the shell is mesoporous silica loaded tungsten oxide, and the movable inner core is noble metal particles. According to the invention, the Yolk-shell structure has a unique cavity nanostructure and the noble metal particle movable core, the movable core provides large-area active sites, and the cavity is used as a nanoreactor to provide a space for catalytic reaction; the mesoporous silica shell protects the internal noble metal particles, so that the loss of the noble metal particles in sintering and reaction is inhibited, and the stability of the catalyst is improved. Moreover, tungsten oxide is uniformly distributed on the surface of mesoporous silica, when glucose is catalyzed to prepare ethylene glycol, glucose molecules form small molecules in a shell layer through reverse aldol condensation, tungsten oxide can promote rapid chain scission of glucose, and the formed small molecules rapidly pass through channels of mesoporous silica so as to be in contact with internal active components to catalyze formation of ethylene glycol through hydrogenation.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a Yolk-shell bifunctional catalyst, a preparation method thereof and an application in the preparation of ethylene glycol by hydrogenolysis of glucose. Background technique [0002] The depletion of fossil fuels and the deterioration of the environment make it inevitable for people to look for new energy sources to adapt to the development of society. Biomass is the most abundant resource on earth, so there is huge potential to use biomass to replace non-renewable energy sources to produce industrial materials and chemicals. Biomass resources can be used to produce small molecular compounds such as levulinic acid (LA), methylfurfural (HMF), formic acid (FA), ethylene glycol (EG) and 1,2-propanediol (1,2-PG). As an important industrial material, EG can be used in the production of antifreeze, polyester resin and fine chemicals. In recent years, with the increasing demand for E...

Claims

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Application Information

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IPC IPC(8): B01J23/652C07C29/00C07C31/20
CPCB01J23/6527C07C29/00C07C31/202Y02P20/52
Inventor 陈超刘悦辛强花周超张治国
Owner QINGDAO UNIV OF SCI & TECH
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