A kind of composite cross-linking agent intelligent hydrogel and its preparation method and application
A composite cross-linking agent and hydrogel technology, which is applied in the direction of pharmaceutical formulations, medical preparations of non-active ingredients, etc., can solve the problems of long response time of gel materials, improve biocompatibility, improve response speed, The effect of improving mechanical properties
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Embodiment 1
[0053] The preparation process of polyethylene glycol diacrylate (PEGDAc) used in Examples 3 to 6 is as follows: Take 6g of PEG and dissolve it in 50ml of dichloromethane, add 1ml of acrylic acid and 0.1g of 2-methylaminopyridine, mix well, and put it under the protection of argon. , another 1g of N,N-dicyclohexylcarbodiimide was dissolved in 20ml of dichloromethane, slowly added to the above solution under ice-cooling, and reacted at room temperature for 48h. The reaction solution was washed once with 1M hydrochloric acid solution, twice with saturated sodium carbonate solution, and three times with distilled water, dried over anhydrous magnesium sulfate, and then rotary evaporated to obtain polyethylene glycol diacrylate, which was designated as PEGDAc. Its H 1 NMR spectrum see figure 1 , resulting in:
[0054] δ=3.58~3.63(t,4H,-OCH 2 CH 2 ); δ=4.31~4.39(m,2H,-CH 2 ); δ=5.77~5.80,6.32~6.4(m,2H,=CH 2 ); δ=6.03~6.11(m,1H,=CH-).
Embodiment 2
[0056] The preparation process of polycaprolactone diacrylate (PCLDAc) used in implementation 3-6 is as follows: take 10g of polycaprolactone diol and dissolve it in 100ml of dichloromethane, add 1g of triethylamine, stir well, and Under protection, another 0.75 g of acryloyl chloride was mixed with 20 ml of dichloromethane, and slowly added dropwise to the above solution under ice bath, and reacted at 40° C. for 24 hours after the dropwise addition was completed. The reaction solution was washed once with 1M hydrochloric acid solution, twice with saturated sodium carbonate solution, and three times with distilled water, dried over anhydrous magnesium sulfate and then rotary evaporated to obtain polycaprolactone diacrylate, which was designated as PCLDAc. Its H 1 NMR spectrum see figure 2 , resulting in:
[0057] δ=1.31~1.35(m,2H,-CH2-);δ=1.58~1.61(m,2H,-CH 2 -); δ=2.26~2.31(m,2H,-CH 2 -); δ=3.8~3.81(t,2H,-CH 2 -C=O); δ=4.05~4.1(t,2H,-CH 2 -O-); δ=5.75~5.78,6.34~6.39(m,...
Embodiment 3
[0059] Weigh 0.0208g of PEGDAc, 0.0291g of PCLDac, and 0.1998g of N-isopropylacrylamide and dissolve them in 2ml of 1,4-dioxane, mix them uniformly by ultrasonication for 15 minutes, add 6mg of azobisisobutylcyanide, mix well and freeze Thaw cycle to remove oxygen, react at 60°C for 24 hours under the protection of argon, crush the reactor, soak the gel in distilled water for 4 days, change the water every day, remove unreacted particles to obtain the composite crosslinking agent intelligent hydrogel, cut into 10mm*5mm cylindrical small pieces are reserved, marked as N1.
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