Crosslinking agent and cross-linked polymer as well as preparation method and application thereof
A technology of cross-linking polymer and cross-linking agent, which is used in the preparation of X-ray contrast agents, inactive ingredients of polymer compounds, pharmaceutical formulations, etc. Stable, wide source of raw materials, adjustable and controllable shape and size
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[0041] Preparation of cross-linked polymer and method for forming cross-linked polymer material
[0042] The cross-linked polymer of the present invention is obtained by mixing a cross-linking agent, a cross-linked macromolecule or a polymer and a catalyst, and then cross-linking and forming at normal temperature or by heating. The catalyst is usually an acid, which can be neutralized with a basic substance or removed under reduced pressure.
[0043] When molding, the crosslinking agent, crosslinked macromolecule or polymer, catalyst and solvent mixture are injected into the mold, and then crosslinked by heating to form a crosslinked polymer material with a specific size and shape. The cross-linked polymer material can be made into particles, microspheres, hydrogels, foam porous materials and the like by existing techniques.
[0044] In addition, in order to make the cross-linked polymer material of the present invention have special curative effect or be used for image obs...
Embodiment 1
[0054] Embodiment one, preparation crosslinking agent
[0055] 1. Preparation of crosslinking agent N,N'-bis(2,2-dimethoxyethyl)succinamide
[0056] Add 20 milliliters of 2-aminodimethylacetal, 34 milliliters of triethylamine and 100 milliliters of chloroform into a 250 milliliter round-bottomed flask, cool to 0-5°C with an ice-water bath, slowly drop in 24 milliliters (1 / 1, V / V) succinoyl chloride / anhydrous chloroform solution, let the temperature rise from 0-5°C to room temperature after dropping, continue to stir for 6-12 hours, evaporate the solvent under reduced pressure, add 300 ml of acetone to disperse Dissolve the solid product, remove the triethylamine salt therein by filtration under reduced pressure, then evaporate the acetone under reduced pressure, and recrystallize and purify the crude solid product 2-3 times with petroleum ether or ethyl acetate, filter to obtain the product, and dry it in vacuo. A white solid product was obtained in >60% yield.
[0057] Aft...
Embodiment 2
[0075] Embodiment two, preparation cross-linked polymer material
[0076] Prepare cross-linked polymer (cross-linked polymer material) with the cross-linking agent of embodiment 1, preparation method example is as follows:
[0077] 1. Preparation of granular polymer materials by crosslinking polyvinyl alcohol with N,N'-bis(2,2-dimethoxyethyl)succinamide
[0078]Heat and dissolve polyvinyl alcohol to prepare 10 ml of 15% aqueous solution, add 50 mg of N,N'-di(2,2-dimethoxyethyl)succinamide crosslinking agent and appropriate amount of dye (such as 4 mg Reactive blue, the role of the dye is to facilitate the distinction and observation), after stirring and dissolving, add 0.2 ml of 10N toluenesulfonic acid solution, stir for 15 minutes, smear on the glass, dry in the air, heat at 80 ° C for 3-6 hour to obtain cross-linked polymers, cross-linked polymers are put into 5% sodium bicarbonate water and soaked for 3-12 hours, taken out, and then soaked and washed with water for 3-5 ti...
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