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

A technology of core-shell catalysts and hollow microspheres, 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 achieve Good catalytic effect, shorten the diffusion time, increase the effect of the outer surface area

Active Publication Date: 2021-10-01
EAST CHINA JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Configure a 1mol / L glucose solution, take 70mL of the solution after it is completely dissolved, place it in a 100mL tetrafluoroethylene-lined reactor, conduct a hydrothermal reaction at 180°C for 5h, and wait until the reactor temperature is cooled to room temperature to obtain Brown product - carbon globules. The obtained product was alternately washed four 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 the reactants tetraethyl orthosilicate, aluminum oxide, tetrapropylammonium hydroxide and deionized water as 25:0.668:9:480, prepare the ZSM-5 precursor with a silicon-aluminum ratio of 25 liquid.

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

Embodiment 2

[0049] The difference with Example 1 is:

[0050] In step (2), according to Al 2 o 3 :TPAOH:TEOS:H 2 The molar ratio of O=0.5:9:25:480 (Si / Al ratio is 50) prepares ZSM-5 precursor solution, obtains Si:Al=50 ZSM-5 hollow microsphere;

[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 load of the double salt is 8wt%.

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

Embodiment 3

[0054] The difference with Example 1 is:

[0055] In step (2), according to Al 2 o 3 :TPAOH:TEOS:H 2 The molar ratio of O=0.333:9:25:480 (Si / Al ratio is 75) prepares ZSM-5 precursor liquid, obtains the ZSM-5 hollow microsphere of Si:Al=75;

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

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

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Abstract

The invention discloses a hollow microsphere core-shell catalyst and a preparation method and an application thereof, and belongs to the field of organic chemical synthesis, and the preparation method comprises the following steps: preparing ZSM-5 hollow microspheres, and preparing ZSM-5 hollow microspheres, pseudo-boehmite and sesbania powder to obtain a ZSM-5 / gamma-Al2O3 hollow microsphere carrier; and respectively dipping the ZSM-5 / Al2O3 hollow microsphere core-shell catalyst in a NaCl solution and an AlCl3 solution, and carrying out a crystallization reaction so as to obtain the NaAlCl4 / ZSM-5 / gamma-Al2O3 hollow microsphere core-shell catalyst. The catalyst provided by the invention has a good catalytic effect on preparation of dimethyl dichlorosilane from disproportionated methyl trichlorosilane and trimethyl chlorosilane, and the yield of dimethyl dichlorosilane at 200 DEG C can reach 73% or 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 its preparation method and application. 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 earth's crust, it is tightly bound to oxygen in the form of silica and metallosilicates. Due to silicon's high silicon-oxygen bond strength 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. Silicone materials have both inorganic and organic characteristics. The complex and changeable structure makes silicone have the characteristics of high pressure resistance, high temperature resistance, corrosion resistance, stain resistance, moisture resistance, water repellency, electrical insulati...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J35/08B01J35/10B01J37/02B01J37/10C07F7/12
CPCB01J37/10B01J37/024B01J29/40C07F7/125B01J2229/42B01J2229/20B01J35/60B01J35/51
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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