Preparation method and application of polymer microsphere with core shell and multi-stage pore structure
A multi-level pore, polymer technology, applied in the preparation of microspheres, microcapsule preparations, chemical instruments and methods, etc., to achieve the effect of promoting hydrolysis and speeding up the etching process
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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 liner, then add DMF and EtOH (V DMF :V EtOH =1:1, 15mL) solution, forming a homogeneous solution. Add 0.2677g Zn(NO3)2·6H2O to the obtained 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 by *). 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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