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

A technology of core-shell catalysts and hollow microspheres, applied in catalyst activation/preparation, catalyst carriers, molecular sieve catalysts, etc., can solve the problems of low catalytic efficiency, low economic benefits, and low catalyst sublimation temperature

Active Publication Date: 2021-09-10
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 influence of it makes it have certain limitations in 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

[0042] (1) Prepare 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 8 hours, and cool the reactor 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.

[0043] (2) Weigh 15g Al(NO 3 ) 3 9H 2 O, add dehydrated alcohol, it is mixed with the aluminum nitrate ethanolic solution of 0.4mol / L. Take 60mL of this solution, add 0.2g of carbon pellets, stir for 1h, and let it fully dissolve. Then pour it into a reaction kettle lined with tetrafluoroethylene, conduct a hydrothermal reaction at 180°C for 6 hours, and cool to room temperature to obtain a black precipitate. After filtering, washing, and drying in an oven at 80°C for 5 hours, Al 2 o 3 A product of @C. Al again 2 o 3 @C is t...

Embodiment 2

[0049] The difference with Example 1 is:

[0050] In step (3), 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 the ZSM-5 precursor solution to obtain γ-Al with Si:Al=50 2 o 3 @ZSM-5 hollow microsphere carrier;

[0051] In step (4), in AlCl 3 The immersion time in the solution is 4h, and the load of double salt is 8wt%.

[0052] Connect the reaction instrument with the gas chromatograph, use the gas chromatograph sampling chamber, vaporize the reactant and enter the reaction kettle, and the reacted product enters the chromatogram for detection and analysis along with the carrier; prepare monomethyltrichlorosilane and trichlorosilane Methyl monochlorosilane volume ratio is the reaction solution of 1:2, the NaAlCl of 0.5g 4 / γ-Al 2 o 3 @ZSM-5 hollow microsphere core-shell catalyst is placed in a single-stage high-temperature furnace reaction tube, the reaction temperature of the high-temperature furnace is adjusted, an...

Embodiment 3

[0055] The difference with Example 1 is:

[0056] In step (3), 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 γ-Al with Si:Al=75 2 o 3 @ZSM-5 hollow microsphere carrier;

[0057] In step (4), in AlCl 3 The immersion time in the solution is 3 hours, and the loading amount of the double salt is 12wt%.

[0058] Connect the reaction instrument with the gas chromatograph, use the gas chromatograph sampling chamber, vaporize the reactant and enter the reaction kettle, and the reacted product enters the chromatogram for detection and analysis along with the carrier; prepare monomethyltrichlorosilane and trichlorosilane Methyl monochlorosilane volume ratio is 1:2 reaction liquid, the NaAlCl of 0.7g 4 / γ-Al 2 o 3 @ZSM-5 hollow microsphere core-shell catalyst is placed in a single-stage high-temperature furnace reaction tube, the reaction temperature of the high-temperature furnace is adjusted, and the re...

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Abstract

The invention discloses a hollow microsphere core-shell catalyst as well as a preparation method and application thereof, and belongs to the technical field of organosilicone, the preparation method comprises the following steps: preparing gamma-Al2O3 hollow microspheres, preparing a ZSM-5 precursor solution from tetraethyl orthosilicate, aluminum oxide, tetrapropylammonium hydroxide and deionized water, and preparing a gamma-Al2O3@ ZSM-5 hollow microsphere carrier from the ZSM-5 precursor solution and the gamma-Al2O3 hollow microspheres; and then respectively dipping in a NaCl solution and an AlCl3 solution, and carrying out a crystallization reaction, so as to obtain the NaAlCl4/gamma-Al2O3 coated ZSM-5 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 70% or above.

Description

technical field [0001] The invention relates to the technical field of organosilicon, 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 insulation,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J37/10B01J37/08B01J35/10B01J37/02B01J32/00C07F7/12
CPCB01J29/40B01J37/10B01J37/082B01J35/1004B01J35/008B01J37/0201C07F7/125B01J2229/18Y02P20/52
Inventor 徐文媛沈蒙莎黄鸿坤程永兵李素颖樊俊杰徐雨
Owner EAST CHINA JIAOTONG UNIVERSITY
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