A kind of preparation method of light-reducing agent dual responsive polyurethane hydrogel
A hydrogel, responsive technology, applied in bandages, absorbent pads, medical science, etc., can solve the problems of complex preparation methods of light-responsive hydrogels, low strength, and few research reports on light-responsive polyurethane hydrogels, etc. Achieving the effects of favorable regulation, low cost and simple preparation method
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[0034] The preparation method of the prepolymer is as follows: Weigh 8.0~9.0g polyethylene glycol and 0.88~1.2mL hexamethylene diisocyanate and add N 2 In the three-necked flask under protection, weigh 40-80mL of anhydrous N,N-dimethylformamide and add it into the three-necked flask, dissolve PEG and HDI under magnetic stirring, heat the system to 80-90°C, and drop into 100 ~200μL stannous octoate catalyst, react for 2~4 hours to obtain prepolymer;
[0035] The preparation method of the cross-linked network is as follows: weigh cyclodextrin (0.05-0.50g), azobenzene (0.008-0.08g) and DSDPDO (0.05-0.50g) in a beaker, add 10-15mL of anhydrous N,N - Dissolve dimethylformamide, add the solution to the prepolymer prepared in the above steps, mix well and pour it into a mold, heat the mold to 80-90°C, and cure the sample for 18-36 hours to obtain a cross-linked polymer The internet;
[0036] The post-treatment method is as follows: soak the cross-linked network in 300-500mL methano...
Embodiment 1
[0041] Thioglycerol (12g, 100mmol) was dissolved in 20mL of methanol, hydrogen peroxide (6.8g, 60mmol, 30wt% aqueous solution) was added dropwise, and stirred at room temperature for 6h after the addition was complete. The solvent was removed by rotary evaporation to obtain a colorless transparent viscous liquid, and the crude product was recrystallized in a mixed solvent of n-hexane / methanol to obtain a white solid DSDPDO (10.0 g, yield 93.2%).
[0042] Dissolve 8.5g of polyethylene glycol (molecular weight 10000g / mol, PDI=1.1) and 0.914mL of hexamethylene diisocyanate in 40mL of anhydrous N,N-dimethylformamide, after heating to 85°C, drop into 140 μL stannous octoate catalyst, reacted for 3 hours to obtain prepolymer; weigh β-cyclodextrin (0.25g), 4-phenylazophenol (0.044g) and DSDPDO (0.25g) and dissolve in 12mL of anhydrous N , in N-dimethylformamide, add the solution to the prepolymer prepared in the above steps, mix well and pour it into a mold, heat to 85°C and cure for...
Embodiment 2
[0044] The preparation method of dithioglycerol (3,3'-disulfane disubstituted dipropyl-1,2-diol, DSDPDO) is consistent with that in Example 1.
[0045] Take by weighing 4-phenylazophenol (4g, 20mmol) and potassium carbonate (8.29g, 60mmol) and dissolve in 50mL acetone, under N 2 Allyl bromide (4.8 g, 40 mmol) was added under protection, and the system was heated until the acetone was refluxed, reacted for 24 h and then cooled to room temperature. The product was filtered to obtain a filtrate, and after concentration, the crude product was recrystallized in n-hexane to obtain tan monovinyl azobenzene (4.36 g, yield 91.5%). Then weighed monovinyl azobenzene (2.38g, 0.01mol), photoinitiator benzoin diethyl ether (DMPA, 0.308g, 0.0012mol) and thioglycerol (1.44g, 0.012mol, 90%) were dissolved in 20mL methanol , freezing-vacuumizing-nitrogen filling, repeated three times, and reacting at room temperature under ultraviolet light for 2 hours. After the reaction, the product was rev...
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