Vinyl modified star-shaped polycaprolactone and synthesis method thereof
A polycaprolactone and vinyl technology, which is applied in the field of vinyl-modified star-shaped polycaprolactone and its synthesis, can solve the problem that the support of parts is difficult to dismantle, it is difficult to meet the personalized customization requirements of fine-structure medical devices, and the precision is low. and other problems, to achieve the effect of good degradability, good biocompatibility and high precision
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Embodiment 1
[0035] Take 15.16g ε-caprolactone (0.105mol), 0.0092g of glycerol (0.1mmol), 105μL stannous octoate in anhydrous toluene solution (0.1mol / L), and add them into a dry polymerization bottle with a magnet in sequence, Then remove the solvent under reduced pressure, and then pass argon, and repeat this 4 times, and finally react the vacuum-sealed polymerization bottle at a constant temperature (120°C) for 48 hours, then dissolve the product with 100mL of dichloromethane, and then use 500mL of ethanol / n-hexane Alkanes (v / v=1:1) were reprecipitated, filtered and dried in vacuo to obtain 13.35 g of three-armed star-shaped polycaprolactone as a white solid, with a yield of 88%.
[0036] Under the protection of nitrogen, dissolve 12g (0.1mmol) three-armed star-shaped polycaprolactone in 100mL of dehydrated tetrahydrofuran, and keep magnetic stirring under ice bath conditions, first add 10.1g (0.1mol, 13.9mL) Triethylamine, and then slowly add 9.1g (0.1mol, 8.2mL) of acryloyl chloride d...
Embodiment 2
[0038] Take 50.05g ε-caprolactone (0.347mol), 0.0136g of pentaerythritol (0.1mmol), and 17.4 μL of anhydrous toluene solution of stannous octoate (0.1mol / L), and add them successively to a dry polymerization bottle with a magnet, and then Remove the solvent under reduced pressure, and then pass argon, and repeat this 4 times. Finally, react the vacuum-sealed polymerization bottle at a constant temperature (140°C) for 72 hours, then dissolve the product with 200mL of dichloromethane, and then use 1000mL of ethanol / n-hexane (v / v=1:1) reprecipitated, filtered and dried in vacuo to obtain 40.05 g of four-armed star-shaped polycaprolactone as a white solid, with a yield of 80%.
[0039] Under the protection of argon, dissolve 10g (0.02mmol) of four-armed star-shaped polycaprolactone in 30mL of dehydrated tetrahydrofuran, and keep magnetic stirring under the condition of ice bath, first add 80.8g (0.8mol, 111.2mL ) triethylamine, and then slowly dropwise added 84g (0.8mol, 86.6mL) o...
Embodiment 3
[0041] Take 20.04g ε-caprolactone (0.139mol), 0.18g cyclohexyl alcohol (1mmol), and 695μL stannous octoate solution in anhydrous toluene (0.1mol / L), add them to a dry polymerization bottle with a magnet in turn, and then Remove the solvent under reduced pressure, and then pass argon, and repeat this 4 times. Finally, react the vacuum-sealed polymerization bottle at a constant temperature (160°C) for 24 hours, then dissolve the product with 150mL of dichloromethane, and then use 750mL of ethanol / n-hexane (v / v=1:1) reprecipitated, filtered and dried in vacuo to obtain 16.98 g of white solid six-armed star-shaped polycaprolactone with a yield of 84%.
[0042]Under the protection of nitrogen, dissolve 10g (0.5mmol) six-armed star-shaped polycaprolactone in 40mL of dehydrated tetrahydrofuran, and keep magnetic stirring under ice bath conditions, first add 1.516g (3.75mmol, 2.08mL) Triethylamine, and then slowly add 1.89g (15mmol) of acrylic anhydride dropwise, during the dropwise a...
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