Hollow microsphere core-shell catalyst and preparation method and application thereof

A technology of core-shell catalysts and hollow microspheres, which is applied in the direction of catalyst activation/preparation, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of being easily affected by carbon deposition, low catalyst sublimation temperature, and low catalytic efficiency, and achieves Good catalytic effect, shorten the diffusion time, increase the effect of the outer surface area

Active Publication Date: 2022-08-05
EAST CHINA JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Previous studies have shown that in the disproportionation reaction, due to AlCl 3 The presence of AlCl greatly reduces the energy barrier required for the reaction and enables the disproportionation reaction to proceed smoothly, but the AlCl 3 The sublimation temperature of the catalyst is low, and it is easy to cause the loss of the catalyst during the reaction process. The economic benefit is low and the catalytic benefit is not high; the ZSM-5 molecular sieve contains Lewis acid and Bronsted acid that catalyze dimethyldichlorosilane, and has certain catalytic activity. , but because it is a silica-alumina material, its catalytic activity is low, and it needs to be modified by loading active components to change the catalytic selectivity and improve stability, and its strong surface Bronsted acid strength makes it susceptible to carbon deposition The impact of it has certain restrictions on the preparation of dimethyldichlorosilane by disproportionation

Method used

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  • Hollow microsphere core-shell catalyst and preparation method and application thereof
  • Hollow microsphere core-shell catalyst and preparation method and application thereof
  • Hollow microsphere core-shell catalyst and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] (1) configure a 1mol / L glucose solution, take 70 mL of this solution after being completely dissolved, place it in a 100 mL tetrafluoroethylene-lined reaction kettle, perform hydrothermal reaction at 180 ° C for 5 h, and wait until the temperature of the reaction kettle is cooled to room temperature to obtain Brown product - carbon pellets. The obtained product was alternately washed 4 times with absolute ethanol and deionized water, dried at 80 °C for 5 h, and then reserved for use.

[0042] (2) According to the molar ratio of reactants ethyl orthosilicate, aluminum oxide, tetrapropylammonium hydroxide and deionized water as 25:0.668:9:480, prepare a ZSM-5 precursor with a silicon-to-aluminum ratio of 25 liquid.

[0043] Take 0.2g of carbon pellets, add it to 20mL of absolute ethanol, then add it to 60mL of ZSM-5 precursor solution, add NaOH, adjust pH=10, stand at room temperature for 8h, filter, wash, and then place it Dry in an oven at 80 °C for 5 h to obtain ZSM-...

Embodiment 2

[0049] The difference from Example 1 is:

[0050] In step (2), according to Al 2 O 3 :TPAOH:TEOS:H 2 O=0.5:9:25:480 (Si / Al ratio is 50) to prepare ZSM-5 precursor solution to obtain ZSM-5 hollow microspheres with Si:Al=50;

[0051] In step (4), in AlCl 3 The immersion time in the solution is 4h, take NaCl and AlCl 3 The masses are 0.0976g and 0.2224g respectively, and the loading amount of the double salt is 8wt%.

[0052] During detection and analysis, the reaction temperature was 180° C., the catalyst amount was 0.5 g, and the ratio of reactants was 1:2, and the yield of dimethyldichlorosilane prepared by disproportionation was 70.68%.

Embodiment 3

[0054] The difference from Example 1 is:

[0055] In step (2), according to Al 2 O 3 :TPAOH:TEOS:H 2 O=0.333:9:25:480 (Si / Al ratio is 75) to prepare ZSM-5 precursor solution to obtain ZSM-5 hollow microspheres with Si:Al=75;

[0056] In step (4), in AlCl 3 The immersion time in the solution was 3h, and NaCl and AlCl were weighed 3 The masses were 0.1464g and 0.3336g respectively, and the loading of the double salt was 12wt%.

[0057] During detection and analysis, the reaction temperature was 240° C., the catalyst amount was 0.7 g, and the ratio of reactants was 1:1, and the yield of dimethyldichlorosilane prepared by disproportionation was 72.26%.

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Abstract

The invention discloses a hollow microsphere core-shell catalyst and a preparation method and application thereof, belonging to the field of organic chemical synthesis, including the preparation of ZSM-5 hollow microspheres, the preparation of ZSM-5 hollow microspheres, pseudo-boehmite and succulent powder get ZSM‑5@γ‑Al 2 O 3 Hollow microsphere carrier; then immersed in NaCl solution and AlCl respectively 3 After the solution, the crystallization reaction gives NaAlCl 4 / ZSM‑5@γ‑Al 2 O 3 Hollow microsphere core-shell catalyst. The catalyst of the invention has good catalytic effect on the preparation of dimethyldichlorosilane by disproportionation of monomethyltrichlorosilane and trimethylmonochlorosilane, and the yield of dimethyldichlorosilane can reach 73 under the condition of 200° C. %above.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a hollow microsphere core-shell catalyst and a preparation method and application thereof. Background technique [0002] The most abundant elements in the Earth's crust are oxygen (49.5%) and silicon (25.7%). However, there is no free silicon in the crust, which is tightly bound to oxygen in the form of silica and metallosilicates. Due to the high silicon-oxygen bond strength of silicon of 108 kCal / mol, it is difficult to separate silicon from oxygen linkages despite its high abundance. It is precisely because of the particularity of its structure that its performance is unique, and the silicone material has both inorganic and organic properties. The complex and changeable structure makes silicones have the characteristics of high pressure resistance, high temperature resistance, corrosion resistance, stain resistance, moisture resistance, water repellency, electrical ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40B01J35/08B01J35/10B01J37/02B01J37/10C07F7/12
CPCB01J35/08B01J37/10B01J35/10B01J37/024B01J29/40C07F7/125B01J2229/42B01J2229/20
Inventor 徐文媛沈蒙莎黄鸿坤程永兵李素颖徐雨樊俊杰
Owner EAST CHINA JIAOTONG UNIVERSITY
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