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Preparation method and application of polymer microspheres with both core-shell and hierarchical pore structures

A multi-level pore, polymer technology, applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., to accelerate the etching process and promote the effect of hydrolysis

Active Publication Date: 2021-08-03
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Few materials with both hierarchical porosity and core-shell structure have been reported so far, and the synthesis by such a simple method is itself a challenge

Method used

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  • Preparation method and application of polymer microspheres with both core-shell and hierarchical pore structures
  • Preparation method and application of polymer microspheres with both core-shell and hierarchical pore structures
  • Preparation method and application of polymer microspheres with both core-shell and hierarchical pore structures

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of Schiff Base Ligand L

[0025] Weigh 0.2683g of 4-amino-3-hydroxybenzoic acid and 0.6126g of terephthalaldehyde into a flask containing 30mL of EtOH, and slowly reflux at 55°C for 6 hours. It can be clearly seen that the colorless mixture gradually turns yellow. Then, a yellow powder solid was obtained by filtration, washed several times with cold ethanol, and then vacuum-dried at 40°C.

Embodiment 2

[0027] Preparation of metal-polymer microspheres with core-shell structure and mesoporous-microporous-macropore hierarchical pore structure.

[0028] Take by weighing 0.0809g ligand L and join in the autoclave of polytetrafluoroethylene lining, then add DMF and EtOH (V DMF :V EtOH =1:1,15mL) solution to form a homogeneous solution. Add 0.2677g Zn(NO3)2•6H2O to the resulting solution, then stir for 10-20 minutes, and finally put the autoclave into an oven and heat at 140°C for 48h. Cool to room temperature, filter with suction to obtain a dark red powder solid, wash with DMF and EtOH three times, and finally dry under vacuum at 60°C overnight.

Embodiment 3

[0030] Schiff base ligand L of the present invention and metal polymer Zn-L-CP 13 C CP / MAS NMR spectra such as figure 1 shown. 13 In the CCP / MAS NMR spectrum, the strong signal of ligand L at 175.7ppm is attributed to the carbon on the carboxyl group connected to the benzene ring in ligand L. The strong signal at 161.6ppm is attributed to the carbon forming the Schiff base, and the strong signal at 156.6ppm is attributed to the carbon connected to the hydroxyl group on the benzene ring. Peaks marked with an asterisk are due to the spin sidebands of the samples (indicated with *). 13 The signals of the metal polymer Zn-L-CP at 178.9ppm, 167.6ppm and 161.6ppm in the C CP / MAS NMR spectrum are due to the downfield of the carboxyl group in the ligand L, the Schiff base, and the hydroxyl group after coordination with Zn2+ Movement, caused by chemical shift increase. This further proves that Zn 2+ Coordination with ligand L was successful.

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Abstract

The present invention relates to the preparation method and application of polymer microspheres with both core-shell and hierarchical pore structures. 3-hydroxy-4-aminobenzoic acid and terephthalaldehyde are refluxed in an ethanol solvent to obtain a Schiff base The ligands of functional groups are purified by solvent and dried in vacuum to obtain a yellow powder. Add the above powder and zinc nitrate hexahydrate into the reactor, add N,N-dimethylformamide and ethanol as solvents, stir well and place Heated in an oven, washed several times with N,N-dimethylformamide and ethanol, and dried overnight in vacuum to prepare metal-polymer microspheres with a core-shell structure and mesoporous-micropore-macropore hierarchical pore structure. Compared with the prior art, the present invention is used as a heterogeneous catalyst to carry out the application of 2-pyridinemethanol acetate deacetylation reaction, the catalyst can be recycled up to 7 times and the reaction yield can still reach 90% stably, without significant loss of its catalytic activity.

Description

technical field [0001] The invention relates to a metal polymer microsphere, in particular to a preparation method and application of a metal polymer microsphere with a core-shell structure and a mesoporous-micropore-macropore level pore structure. Background technique [0002] As an important functional polymer material, polymer microspheres have received more and more attention in various fields such as catalytic carriers, drug delivery, enzyme immobilization, controlled release, adsorption and separation due to their unique porous properties. [0003] The core-shell structure material is a composite material with a self-assembled structure formed by chemical bonds or other interactions, and generally consists of a central core and an outer shell. Polymers with a core-shell structure can not only prevent agglomeration but also enhance the selectivity and activity of the reaction. Its synthesis is considered to be one of the most convenient and effective methods to obtain n...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J13/02B01J31/06C07D213/64
CPCB01J13/02B01J31/06C07D213/64C08G83/008Y02P20/584
Inventor 郭建宇周亚芳
Owner SHANGHAI NORMAL UNIVERSITY