A kind of visible polyhydroxy polymer embolization microsphere and preparation method thereof
A technology for embolizing microspheres and polymers, applied in the field of medical materials, can solve the problems of increased difficulty, cumbersome operation steps, vascular stimulation, etc., and achieves the effects of simple and easy operation, reduced surgical risks, and good scalability
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Embodiment 1
[0037]
[0038] Slowly add 50 mL of dimethyl sulfoxide solution containing 419.0 g of 3,5-diiodo-4-aminobenzaldehyde dimethyl acetal into a four-necked reaction flask filled with aqueous sodium hydroxide solution (40 g, 300 mL), and stir to make the solution Uniform; Acryloyl chloride (99.5g) was slowly added dropwise, and the reaction was continued for 1 hour after the dropwise addition. Then add saturated sodium chloride solution (100mL) to the above solution, add ethyl acetate (2×200mL) for extraction, wash the organic phase with water (2×100mL), and concentrate the organic phase to obtain crude product purified by column chromatography to obtain Yellow oily product 3,5-diiodo-4-acrylamidobenzaldehyde dimethyl acetal 1 (300g), HPLC purity 99.0%, 1 HNMR [DMSO-d 6 ]:8.201(s,1H),7.541(s,2H),6.482-6.410(m,1H),6.172-6.124(m,1H),5.714-5.682(m,1H),5.490(s,1H), 3.252(s,6H).
Embodiment 2
[0040]
[0041] In a 2L four-necked reaction flask, add 1000g of water and a molecular weight of 5×10 4 ~8×10 4 150g of polyvinyl alcohol, heated to 96°C for 4 hours, cooled the fully dissolved polyvinyl alcohol solution to room temperature, and added 15.7g of 3,5-diiodo-4-acrylamidobenzaldehyde dimethyl acetal Dimethyl sulfoxide solution 10mL, concentrated hydrochloric acid 100mL, reacted for 3 hours, after the reaction was completed, 560g of 2.5M sodium hydroxide solution was added, and the collected crude product was concentrated to obtain 550g of a gel-like functionalized macromolecular intermediate with a viscosity of 3000cps. This intermediate 2 was kept for future use.
Embodiment 3
[0043]
[0044] In a 2L reaction flask, add sodium 2-acrylamide-2-methylpropanesulfonate (20.0g), potassium persulfate (12.0g) and water, mix and stir until the potassium persulfate is completely dissolved, and then add it into the functionalized The macromolecular intermediate (400g) was stirred evenly to obtain a macromolecular monomer solution, which was placed for subsequent use. Add butyl acetate (2.5L) and ethyl acetate solution (35g) of 10% butyl acetate cellulose in 5L reactor, feed nitrogen, system temperature rises to 63 ℃, add above-mentioned macromolecular monomer solution and four Methylethylenediamine (20 mL), then the reaction was stirred at 58°C for 3 hours. After the reaction, the reaction mixture was washed with butyl acetate and acetone successively, filtered with suction, and dried in vacuum to obtain polyvinyl alcohol embolism microspheres 3 (80 g).
[0045] After swelling and sieving, the embolism microspheres are round and plump, with smooth surface,...
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