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SiO2@metal-organic nanosheet core-shell material, preparation process and catalytic performance detection method

A nanosheet and core-shell technology, applied in the field of materials engineering and catalysts, can solve the problems of small overall size, small size and thickness, and low recycling rate, and achieve the effects of low cost, simple operation, and improved catalytic conversion efficiency

Active Publication Date: 2021-12-21
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Nevertheless, well-exfoliated nanosheets usually have a thickness as low as 1 nm and a very small overall size, and are mostly dispersed in solution as colloids, so as heterogeneous catalytic materials, their recycling rate is low; in addition, although MOFs nano However, due to the small size and thickness, how to further improve the effective collision between substrate molecules and nanosheets has also become a concern.

Method used

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  • SiO2@metal-organic nanosheet core-shell material, preparation process and catalytic performance detection method
  • SiO2@metal-organic nanosheet core-shell material, preparation process and catalytic performance detection method
  • SiO2@metal-organic nanosheet core-shell material, preparation process and catalytic performance detection method

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Experimental program
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Effect test

Embodiment 1

[0103] Take 50 mg of carboxyl-functionalized silica spheres and 10 mg of zirconium tetrachloride and disperse them in 34.5 mL of DMF. After ultrasonic dissolution, add 1 mL of deionized water and 4.5 mL of formic acid. Shake at 120°C for 24 hours. Then add 154 mg of tricarboxylic acid ligand, and continue shaking at 120 °C for 48 h; after the shaking is over, centrifuge to remove the supernatant, wash with deionized water three times, and dry in vacuum at 60 °C for 24 h to obtain a spherical silicon-based metal-organic composite Material. After shaking, the supernatant was removed by centrifugation, washed three times with deionized water, and dried in vacuum at 60°C for 24 hours to obtain spherical SiO 2 @metal-organic nanosheet core-shell materials. Through the ICP test, the content of Zr is 1.63%, and the calculated mass percentage of MOF nanosheet material is 17.7%.

Embodiment 2

[0105] Take 45 mg of carboxyl-functionalized silica spheres and 10 mg of zirconium tetrachloride and disperse them in 34.5 mL of DMF. After ultrasonic dissolution, add 1 mL of deionized water and 4.5 mL of formic acid. Shake at 120°C for 24 hours. Then add 154 mg of tricarboxylic acid ligand, and continue shaking at 120 °C for 48 h; after the shaking is over, centrifuge to remove the supernatant, wash with deionized water three times, and dry in vacuum at 60 °C for 24 h to obtain a spherical silicon-based metal-organic composite Material. After shaking, the supernatant was removed by centrifugation, washed three times with deionized water, and dried in vacuum at 60°C for 24 hours to obtain spherical SiO 2 @metal-organic nanosheet core-shell materials. Through the ICP test, the content of Zr is 2.33%, and the calculated mass percentage of MOF nanosheet material is 25.1%.

Embodiment 3

[0107] Take 50 mg of carboxyl-functionalized silica spheres and 10 mg of zirconium tetrachloride and disperse them in 34.5 mL of DMF. After ultrasonic dissolution, add 1 mL of deionized water and 4.5 mL of formic acid. Shake at 110°C for 24 hours. Then add 150 mg of tricarboxylic acid ligand, and continue shaking at 110 °C for 48 h; after the shaking is over, centrifuge to remove the supernatant, wash with deionized water three times, and vacuum dry at 60 °C for 24 h to obtain a spherical silicon-based metal-organic composite Material. After shaking, the supernatant was removed by centrifugation, washed three times with deionized water, and dried in vacuum at 60°C for 24 hours to obtain spherical SiO 2 @metal-organic nanosheet core-shell materials. Through the ICP test, the content of Zr is 1.06%, and the calculated mass percentage of MOF nanosheet material is 10.5%.

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Abstract

The invention discloses a SiO2@metal-organic nanosheet core-shell material, a preparation process and a catalytic performance detection method. The preparation method comprises the following steps: (1) by taking a silicon dioxide sphere as a carrier, modifying a carboxylic acid functional group on the surface of the silicon sphere through 3-aminopropyl silane and succinic anhydride; (2) adding carboxylic acid silicon balls into a reaction solution for preparing the zirconium-based nanosheet based on the 1, 3, 5-tri (4-carboxyl phenyl) benzene through an in-situ synthesis method, and realizing loading of the nanosheet on the silicon balls through coordination of carboxylic acid; wherein the prepared composite material is prepared from the following parts in percentage by mass: 74.9 to 89.5% of silicon spheres and 10.5 to 25.1% of MOF nanosheet material.

Description

technical field [0001] The invention relates to material engineering and catalyst technology, in particular to a SiO 2 @ Metal-organic nanosheet core-shell material, preparation process and catalytic performance testing method. Background technique [0002] Ultrathin two-dimensional metal-organic nanosheets (MOFs nanosheets), as an emerging class of highly crystalline porous materials, have broad potential due to their ultrathin thickness, large specific surface area, and abundant active sites distributed on the surface. application, in recent years more and more people's attention (C.Tan, X.Cao, X.J.Wu, Q.He, J.Yang, X.Zhang, J.Chen, W.Zhao, S.Han, G.H.Nam , M. Sindoro, and H. Zhang, Chem. Rev. 2017, 18 117, 6225). In particular, studies have shown that MOFs nanosheets exhibit very high activity and mass transfer rates as catalysts (C.Tan, G.Liu, H.Li, Y.Cui, Y.Liu, Dalton Transactions, 2020, 49, 11073) . In the catalytic process of nanosheets, the reactants interact wi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22G01N31/10C07C45/46C07C49/84
CPCB01J31/2239G01N31/10C07C45/46B01J2531/48B01J2231/4205B01J35/397C07C49/84Y02E60/10
Inventor 谭春霞刘国华王永杰程探宇刘锐
Owner SHANGHAI NORMAL UNIVERSITY
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